# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2014

  
data_f_seino_1-butene_twin_36_ss151 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C8 O48 Si24' 
_chemical_formula_weight          1538.2
  
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' 
 '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' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    13.467(8) 
_cell_length_b                    20.219(11) 
_cell_length_c                    19.994(11) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.088(8) 
_cell_angle_gamma                 90.00 
_cell_volume                      5444(5) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.15 
_exptl_crystal_size_mid           0.12 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.896 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3136 
_exptl_absorpt_coefficient_mu     0.669 
_exptl_absorpt_correction_type    Analytical 
_exptl_absorpt_correction_T_min   0.9087 
_exptl_absorpt_correction_T_max   0.9478 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       296(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   'Bruker P4' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             64115 
_diffrn_reflns_av_R_equivalents   0.1028 
_diffrn_reflns_av_sigmaI/netI     0.1273 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        26 
_diffrn_reflns_limit_l_min        -26 
_diffrn_reflns_limit_l_max        25 
_diffrn_reflns_theta_min          1.43 
_diffrn_reflns_theta_max          28.71 
_reflns_number_total              13341 
_reflns_number_gt                 5700 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker XSCANS' 
_computing_cell_refinement        'Bruker XSCANS' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_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)+(0.0479P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none 
_refine_ls_hydrogen_treatment     none 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          13341 
_refine_ls_number_parameters      698 
_refine_ls_number_restraints      15 
_refine_ls_R_factor_all           0.1345 
_refine_ls_R_factor_gt            0.0498 
_refine_ls_wR_factor_ref          0.1347 
_refine_ls_wR_factor_gt           0.1125 
_refine_ls_goodness_of_fit_ref    0.835 
_refine_ls_restrained_S_all       0.841 
_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 
C101 C 0.016(3) 0.477(2) 0.4741(17) 0.148(16) Uiso 0.50 1 d PD . 1 
C102 C -0.022(4) 0.480(2) 0.5369(17) 0.25(3) Uiso 0.50 1 d PD . 1 
C103 C -0.011(3) 0.522(2) 0.5945(18) 0.21(2) Uiso 0.50 1 d PD . 1 
C104 C 0.027(7) 0.505(4) 0.666(2) 0.52(6) Uiso 0.50 1 d PD A 1 
C204 C 0.600(4) 0.008(3) 0.268(2) 0.39(3) Uiso 0.50 1 d PD B 2 
C203 C 0.511(3) -0.001(3) 0.3144(18) 0.29(3) Uiso 0.50 1 d PD B 2 
C202 C 0.511(3) 0.0019(19) 0.3901(17) 0.180(17) Uiso 0.50 1 d PD B 2 
C201 C 0.477(3) -0.0054(19) 0.4533(16) 0.170(16) Uiso 0.50 1 d PD . 2 
C301 C 0.808(3) 0.9220(15) 0.249(3) 0.58(3) Uiso 1 1 d D C 3 
C302 C 0.855(2) 0.8641(12) 0.256(2) 0.332(12) Uiso 1 1 d D C 3 
C303 C 0.8919(15) 0.8003(11) 0.2409(15) 0.247(9) Uiso 1 1 d D C 3 
C304 C 0.8494(18) 0.7338(10) 0.248(2) 0.342(13) Uiso 1 1 d D C 3 
Si16 Si 0.53036(17) 0.62178(11) 0.93640(13) 0.0161(5) Uani 1 1 d . . . 
Si1 Si 0.67325(18) 0.57874(11) 1.05680(14) 0.0160(5) Uani 1 1 d . . . 
Si2 Si 0.82436(19) 0.68949(12) 1.02988(11) 0.0182(5) Uani 1 1 d . . . 
Si3 Si 1.04321(17) 0.72064(11) 1.06198(14) 0.0184(5) Uani 1 1 d . . . 
Si4 Si 1.03298(17) 0.87694(11) 1.06275(13) 0.0154(5) Uani 1 1 d . . . 
Si5 Si 0.82042(19) 0.92558(11) 1.02819(11) 0.0152(5) Uani 1 1 d . . . 
Si6 Si 0.67879(17) 0.80905(11) 1.05717(13) 0.0166(5) Uani 1 1 d . . . 
Si7 Si 0.6772(2) 0.57581(11) 0.82861(13) 0.0163(5) Uani 1 1 d . . . 
Si8 Si 0.81980(17) 0.68992(12) 0.87219(12) 0.0157(5) Uani 1 1 d . . . 
Si9 Si 1.03234(18) 0.72595(12) 0.82496(12) 0.0165(6) Uani 1 1 d . . . 
Si10 Si 1.03002(19) 0.87996(12) 0.82492(12) 0.0181(6) Uani 1 1 d . . . 
Si11 Si 0.82005(19) 0.92886(11) 0.87009(13) 0.0158(5) Uani 1 1 d . . . 
Si12 Si 0.68226(18) 0.81102(12) 0.83100(12) 0.0166(5) Uani 1 1 d . . . 
Si13 Si 0.66339(17) 0.57393(11) 0.44204(14) 0.0162(5) Uani 1 1 d . . . 
Si14 Si 0.80950(18) 0.68988(13) 0.47176(11) 0.0168(5) Uani 1 1 d . . . 
Si15 Si 1.02885(16) 0.72165(11) 0.43861(13) 0.0163(5) Uani 1 1 d . . . 
Si17 Si 0.81686(19) 0.92923(11) 0.47213(11) 0.0139(5) Uani 1 1 d . . . 
Si18 Si 0.67668(18) 0.81348(11) 0.43821(13) 0.0164(5) Uani 1 1 d . . . 
Si19 Si 0.68005(19) 0.57640(11) 0.67262(12) 0.0162(6) Uani 1 1 d . . . 
Si20 Si 0.82262(18) 0.68940(12) 0.63032(13) 0.0183(5) Uani 1 1 d . . . 
Si21 Si 1.03783(18) 0.72611(12) 0.66964(12) 0.0169(6) Uani 1 1 d . . . 
Si22 Si 1.03346(18) 0.88090(12) 0.67127(12) 0.0178(6) Uani 1 1 d . . . 
Si23 Si 0.8199(2) 0.92905(11) 0.62998(13) 0.0167(5) Uani 1 1 d . . . 
Si24 Si 0.69213(18) 0.80958(12) 0.67692(11) 0.0176(5) Uani 1 1 d . . . 
O1 O 0.7683(4) 0.6245(3) 1.0554(4) 0.0364(17) Uani 1 1 d . . . 
O2 O 0.9318(4) 0.6923(3) 1.0626(3) 0.0313(15) Uani 1 1 d . . . 
O3 O 1.0429(5) 0.7991(3) 1.0540(4) 0.0430(16) Uani 1 1 d . . . 
O4 O 0.9189(4) 0.8980(3) 1.0643(3) 0.0318(15) Uani 1 1 d . . . 
O5 O 0.7262(4) 0.8814(3) 1.0498(4) 0.0295(15) Uani 1 1 d . . . 
O6 O 0.7636(4) 0.7542(3) 1.0505(4) 0.0438(18) Uani 1 1 d . . . 
O7 O 0.7678(5) 0.6257(3) 0.8442(4) 0.041(2) Uani 1 1 d . . . 
O8 O 0.9272(4) 0.6944(3) 0.8367(3) 0.0370(16) Uani 1 1 d . . . 
O9 O 1.0282(5) 0.8035(3) 0.8446(3) 0.0315(17) Uani 1 1 d . . . 
O10 O 0.9207(5) 0.9097(3) 0.8340(3) 0.0349(17) Uani 1 1 d . . . 
O11 O 0.7326(5) 0.8808(3) 0.8476(3) 0.0313(17) Uani 1 1 d . . . 
O12 O 0.7552(5) 0.7536(3) 0.8552(3) 0.045(2) Uani 1 1 d . . . 
O13 O 0.8326(5) 0.6851(3) 0.9509(3) 0.0518(19) Uani 1 1 d . . . 
O14 O 0.8349(4) 0.9223(3) 0.9487(3) 0.0362(15) Uani 1 1 d . . . 
O15 O 0.6164(5) 0.5851(3) 1.1257(3) 0.0353(18) Uani 1 1 d . . . 
O16 O 0.6017(5) 0.5994(3) 0.9963(3) 0.045(2) Uani 1 1 d . . . 
O17 O 0.5801(4) 0.5979(3) 0.8671(3) 0.0273(15) Uani 1 1 d . . . 
O18 O 0.6292(4) 0.8036(3) 1.1295(3) 0.0271(14) Uani 1 1 d . . . 
O19 O 0.5939(5) 0.7984(3) 1.0022(3) 0.0396(17) Uani 1 1 d . . . 
O20 O 0.5799(4) 0.8035(3) 0.8716(3) 0.0327(15) Uani 1 1 d . . . 
O21 O 0.7973(4) 0.9995(2) 1.0532(3) 0.0280(15) Uani 1 1 d . . . 
O22 O 0.7902(5) 1.0029(3) 0.8507(3) 0.0276(16) Uani 1 1 d . . . 
O23 O 0.6525(3) 0.57720(19) 0.7496(4) 0.0312(10) Uani 1 1 d . . . 
O24 O 0.6571(3) 0.8049(2) 0.7536(3) 0.0294(10) Uani 1 1 d . . . 
O25 O 1.0602(3) 0.71656(17) 0.7485(3) 0.0259(10) Uani 1 1 d . . . 
O26 O 1.0641(3) 0.88985(18) 0.7480(4) 0.0244(10) Uani 1 1 d . . . 
O27 O 0.7558(4) 0.6244(3) 0.4449(4) 0.0402(18) Uani 1 1 d . . . 
O28 O 0.9220(4) 0.6890(3) 0.4445(3) 0.0292(14) Uani 1 1 d . . . 
O29 O 1.0172(5) 0.7998(3) 0.4363(3) 0.0453(18) Uani 1 1 d . . . 
O30 O 0.9250(4) 0.9125(3) 0.4420(4) 0.0360(16) Uani 1 1 d . . . 
O31 O 0.7358(4) 0.8814(3) 0.4388(3) 0.0273(15) Uani 1 1 d . . . 
O32 O 0.7544(4) 0.7534(3) 0.4428(3) 0.0368(16) Uani 1 1 d . . . 
O33 O 0.7721(5) 0.6233(3) 0.6589(3) 0.0333(18) Uani 1 1 d . . . 
O34 O 0.9379(4) 0.6882(3) 0.6482(3) 0.0255(14) Uani 1 1 d . . . 
O35 O 1.0258(5) 0.8025(3) 0.6522(3) 0.0338(17) Uani 1 1 d . . . 
O36 O 0.9282(5) 0.9143(3) 0.6568(3) 0.048(2) Uani 1 1 d . . . 
O37 O 0.7399(5) 0.8799(3) 0.6639(3) 0.042(2) Uani 1 1 d . . . 
O38 O 0.7724(5) 0.7532(3) 0.6649(3) 0.0414(18) Uani 1 1 d . . . 
O39 O 0.8073(5) 0.6939(3) 0.5514(3) 0.0526(18) Uani 1 1 d . . . 
O40 O 0.8178(5) 0.9190(3) 0.5505(3) 0.0407(17) Uani 1 1 d . . . 
O41 O 0.6082(5) 0.5811(3) 0.3707(3) 0.0343(17) Uani 1 1 d . . . 
O42 O 0.5854(5) 0.5889(3) 0.5009(3) 0.0330(16) Uani 1 1 d . . . 
O43 O 0.5838(4) 0.6022(3) 0.6320(3) 0.0317(16) Uani 1 1 d . . . 
O44 O 0.6146(4) 0.8110(3) 0.3704(3) 0.0273(14) Uani 1 1 d . . . 
O45 O 0.6040(5) 0.8117(3) 0.5015(3) 0.0352(16) Uani 1 1 d . . . 
O46 O 1.0954(4) 0.7006(3) 1.1306(3) 0.0418(18) Uani 1 1 d . . . 
O47 O 0.7905(4) 1.0039(3) 0.4551(3) 0.0227(15) Uani 1 1 d . . . 
O48 O 0.7901(5) 1.0043(3) 0.6489(3) 0.0321(17) Uani 1 1 d . . . 
  
  
_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 
C101 C102 0.90(5) 3_566 ? 
C101 C102 1.359(18) . ? 
C101 C103 1.37(6) 3_566 ? 
C101 C101 1.45(6) 3_566 ? 
C102 C101 0.90(5) 3_566 ? 
C102 C103 1.446(19) . ? 
C102 C102 1.79(7) 3_566 ? 
C103 C101 1.37(6) 3_566 ? 
C103 C104 1.56(2) . ? 
C204 C203 1.523(19) . ? 
C203 C202 1.515(18) . ? 
C202 C201 1.353(18) . ? 
C201 C201 1.98(6) 3_656 ? 
C301 C302 1.341(18) . ? 
C302 C303 1.415(16) . ? 
C303 C304 1.467(16) . ? 
Si16 O30 1.582(6) 4_576 ? 
Si16 O29 1.595(6) 4_576 ? 
Si16 O16 1.599(6) . ? 
Si16 O17 1.615(6) . ? 
Si1 O1 1.580(6) . ? 
Si1 O15 1.582(6) . ? 
Si1 O16 1.601(6) . ? 
Si1 O47 1.607(5) 2_646 ? 
Si2 O13 1.587(6) . ? 
Si2 O2 1.588(6) . ? 
Si2 O6 1.597(6) . ? 
Si2 O1 1.599(6) . ? 
Si3 O46 1.593(6) . ? 
Si3 O3 1.595(6) . ? 
Si3 O45 1.601(6) 4_676 ? 
Si3 O2 1.606(6) . ? 
Si4 O42 1.584(6) 4_676 ? 
Si4 O3 1.589(6) . ? 
Si4 O4 1.595(6) . ? 
Si4 O43 1.599(6) 4_676 ? 
Si5 O14 1.603(7) . ? 
Si5 O21 1.607(6) . ? 
Si5 O4 1.608(6) . ? 
Si5 O5 1.611(6) . ? 
Si6 O6 1.598(6) . ? 
Si6 O18 1.599(6) . ? 
Si6 O19 1.599(6) . ? 
Si6 O5 1.603(6) . ? 
Si7 O48 1.577(6) 2_646 ? 
Si7 O17 1.582(6) . ? 
Si7 O7 1.612(7) . ? 
Si7 O23 1.615(8) . ? 
Si8 O7 1.578(6) . ? 
Si8 O13 1.585(6) . ? 
Si8 O12 1.590(6) . ? 
Si8 O8 1.615(6) . ? 
Si9 O8 1.570(6) . ? 
Si9 O25 1.587(7) . ? 
Si9 O44 1.615(6) 4_676 ? 
Si9 O9 1.617(6) . ? 
Si10 O9 1.596(6) . ? 
Si10 O10 1.601(6) . ? 
Si10 O41 1.602(6) 4_676 ? 
Si10 O26 1.618(7) . ? 
Si11 O10 1.584(6) . ? 
Si11 O14 1.589(7) . ? 
Si11 O11 1.591(6) . ? 
Si11 O22 1.599(6) . ? 
Si12 O24 1.589(7) . ? 
Si12 O12 1.596(6) . ? 
Si12 O11 1.599(6) . ? 
Si12 O20 1.607(6) . ? 
Si13 O21 1.598(5) 2_646 ? 
Si13 O42 1.607(7) . ? 
Si13 O27 1.610(6) . ? 
Si13 O41 1.613(7) . ? 
Si14 O32 1.592(6) . ? 
Si14 O39 1.595(6) . ? 
Si14 O27 1.601(6) . ? 
Si14 O28 1.610(6) . ? 
Si15 O28 1.588(6) . ? 
Si15 O29 1.589(6) . ? 
Si15 O20 1.591(6) 4_675 ? 
Si15 O19 1.595(6) 4_675 ? 
Si17 O40 1.580(7) . ? 
Si17 O47 1.589(6) . ? 
Si17 O31 1.603(6) . ? 
Si17 O30 1.613(6) . ? 
Si18 O31 1.587(6) . ? 
Si18 O44 1.593(6) . ? 
Si18 O45 1.601(6) . ? 
Si18 O32 1.606(6) . ? 
Si19 O23 1.584(8) . ? 
Si19 O33 1.585(6) . ? 
Si19 O22 1.608(6) 2_646 ? 
Si19 O43 1.616(6) . ? 
Si20 O34 1.593(6) . ? 
Si20 O39 1.594(6) . ? 
Si20 O33 1.605(6) . ? 
Si20 O38 1.612(6) . ? 
Si21 O18 1.588(6) 4_675 ? 
Si21 O35 1.591(6) . ? 
Si21 O34 1.606(6) . ? 
Si21 O25 1.615(7) . ? 
Si22 O36 1.596(7) . ? 
Si22 O15 1.598(6) 4_675 ? 
Si22 O26 1.599(7) . ? 
Si22 O35 1.635(6) . ? 
Si23 O36 1.582(7) . ? 
Si23 O40 1.603(7) . ? 
Si23 O37 1.615(7) . ? 
Si23 O48 1.618(6) . ? 
Si24 O37 1.582(7) . ? 
Si24 O38 1.590(6) . ? 
Si24 O24 1.607(7) . ? 
Si24 O46 1.610(6) 4_575 ? 
O15 Si22 1.598(6) 4_576 ? 
O18 Si21 1.588(6) 4_576 ? 
O19 Si15 1.595(6) 4_576 ? 
O20 Si15 1.591(6) 4_576 ? 
O21 Si13 1.598(5) 2_656 ? 
O22 Si19 1.608(6) 2_656 ? 
O29 Si16 1.595(6) 4_675 ? 
O30 Si16 1.583(6) 4_675 ? 
O41 Si10 1.602(6) 4_575 ? 
O42 Si4 1.583(6) 4_575 ? 
O43 Si4 1.599(6) 4_575 ? 
O44 Si9 1.615(6) 4_575 ? 
O45 Si3 1.601(6) 4_575 ? 
O46 Si24 1.611(6) 4_676 ? 
O47 Si1 1.607(5) 2_656 ? 
O48 Si7 1.577(6) 2_656 ? 
  
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 
C102 C101 C102 103(5) 3_566 . ? 
C102 C101 C103 76(4) 3_566 3_566 ? 
C102 C101 C103 155(4) . 3_566 ? 
C102 C101 C101 66(4) 3_566 3_566 ? 
C102 C101 C101 37(2) . 3_566 ? 
C103 C101 C101 134(5) 3_566 3_566 ? 
C101 C102 C101 77(5) 3_566 . ? 
C101 C102 C103 67(4) 3_566 . ? 
C101 C102 C103 136(4) . . ? 
C101 C102 C102 48(3) 3_566 3_566 ? 
C101 C102 C102 29.3(19) . 3_566 ? 
C103 C102 C102 110(4) . 3_566 ? 
C101 C103 C102 37(2) 3_566 . ? 
C101 C103 C104 159(5) 3_566 . ? 
C102 C103 C104 129(4) . . ? 
C202 C203 C204 127(3) . . ? 
C201 C202 C203 158(4) . . ? 
C202 C201 C201 139(4) . 3_656 ? 
C301 C302 C303 159(5) . . ? 
C302 C303 C304 133(2) . . ? 
O30 Si16 O29 109.6(3) 4_576 4_576 ? 
O30 Si16 O16 111.1(4) 4_576 . ? 
O29 Si16 O16 110.4(4) 4_576 . ? 
O30 Si16 O17 107.6(4) 4_576 . ? 
O29 Si16 O17 110.0(4) 4_576 . ? 
O16 Si16 O17 108.0(4) . . ? 
O1 Si1 O15 111.2(4) . . ? 
O1 Si1 O16 108.7(4) . . ? 
O15 Si1 O16 110.2(4) . . ? 
O1 Si1 O47 107.6(3) . 2_646 ? 
O15 Si1 O47 110.6(3) . 2_646 ? 
O16 Si1 O47 108.4(4) . 2_646 ? 
O13 Si2 O2 110.4(4) . . ? 
O13 Si2 O6 109.8(4) . . ? 
O2 Si2 O6 109.3(4) . . ? 
O13 Si2 O1 107.8(4) . . ? 
O2 Si2 O1 109.1(3) . . ? 
O6 Si2 O1 110.4(4) . . ? 
O46 Si3 O3 109.9(4) . . ? 
O46 Si3 O45 108.8(4) . 4_676 ? 
O3 Si3 O45 109.3(4) . 4_676 ? 
O46 Si3 O2 108.2(4) . . ? 
O3 Si3 O2 110.7(3) . . ? 
O45 Si3 O2 109.8(4) 4_676 . ? 
O42 Si4 O3 108.0(4) 4_676 . ? 
O42 Si4 O4 109.2(4) 4_676 . ? 
O3 Si4 O4 110.3(3) . . ? 
O42 Si4 O43 111.7(4) 4_676 4_676 ? 
O3 Si4 O43 108.7(4) . 4_676 ? 
O4 Si4 O43 108.9(4) . 4_676 ? 
O14 Si5 O21 111.8(3) . . ? 
O14 Si5 O4 109.2(3) . . ? 
O21 Si5 O4 110.1(3) . . ? 
O14 Si5 O5 109.8(4) . . ? 
O21 Si5 O5 106.2(3) . . ? 
O4 Si5 O5 109.6(3) . . ? 
O6 Si6 O18 109.2(4) . . ? 
O6 Si6 O19 111.1(4) . . ? 
O18 Si6 O19 108.3(4) . . ? 
O6 Si6 O5 109.9(3) . . ? 
O18 Si6 O5 108.2(4) . . ? 
O19 Si6 O5 110.1(4) . . ? 
O48 Si7 O17 110.5(4) 2_646 . ? 
O48 Si7 O7 107.9(4) 2_646 . ? 
O17 Si7 O7 110.8(4) . . ? 
O48 Si7 O23 110.6(3) 2_646 . ? 
O17 Si7 O23 107.5(3) . . ? 
O7 Si7 O23 109.5(3) . . ? 
O7 Si8 O13 110.4(4) . . ? 
O7 Si8 O12 110.4(4) . . ? 
O13 Si8 O12 108.7(4) . . ? 
O7 Si8 O8 106.8(4) . . ? 
O13 Si8 O8 110.1(3) . . ? 
O12 Si8 O8 110.6(4) . . ? 
O8 Si9 O25 108.1(3) . . ? 
O8 Si9 O44 110.2(3) . 4_676 ? 
O25 Si9 O44 108.9(3) . 4_676 ? 
O8 Si9 O9 109.0(4) . . ? 
O25 Si9 O9 111.0(3) . . ? 
O44 Si9 O9 109.6(3) 4_676 . ? 
O9 Si10 O10 108.8(4) . . ? 
O9 Si10 O41 110.2(3) . 4_676 ? 
O10 Si10 O41 110.8(4) . 4_676 ? 
O9 Si10 O26 111.0(3) . . ? 
O10 Si10 O26 108.9(3) . . ? 
O41 Si10 O26 107.2(3) 4_676 . ? 
O10 Si11 O14 108.9(4) . . ? 
O10 Si11 O11 110.8(4) . . ? 
O14 Si11 O11 108.6(4) . . ? 
O10 Si11 O22 109.5(4) . . ? 
O14 Si11 O22 110.5(3) . . ? 
O11 Si11 O22 108.6(4) . . ? 
O24 Si12 O12 111.7(3) . . ? 
O24 Si12 O11 111.1(3) . . ? 
O12 Si12 O11 108.6(4) . . ? 
O24 Si12 O20 107.6(3) . . ? 
O12 Si12 O20 107.8(4) . . ? 
O11 Si12 O20 110.0(4) . . ? 
O21 Si13 O42 110.5(4) 2_646 . ? 
O21 Si13 O27 109.8(3) 2_646 . ? 
O42 Si13 O27 111.1(4) . . ? 
O21 Si13 O41 106.8(3) 2_646 . ? 
O42 Si13 O41 109.2(4) . . ? 
O27 Si13 O41 109.2(4) . . ? 
O32 Si14 O39 108.2(4) . . ? 
O32 Si14 O27 109.6(4) . . ? 
O39 Si14 O27 111.6(4) . . ? 
O32 Si14 O28 108.9(3) . . ? 
O39 Si14 O28 110.9(3) . . ? 
O27 Si14 O28 107.6(3) . . ? 
O28 Si15 O29 109.1(3) . . ? 
O28 Si15 O20 108.8(4) . 4_675 ? 
O29 Si15 O20 109.6(4) . 4_675 ? 
O28 Si15 O19 109.3(4) . 4_675 ? 
O29 Si15 O19 109.3(4) . 4_675 ? 
O20 Si15 O19 110.6(3) 4_675 4_675 ? 
O40 Si17 O47 109.8(3) . . ? 
O40 Si17 O31 109.7(3) . . ? 
O47 Si17 O31 109.4(3) . . ? 
O40 Si17 O30 109.7(4) . . ? 
O47 Si17 O30 108.7(3) . . ? 
O31 Si17 O30 109.5(4) . . ? 
O31 Si18 O44 107.2(3) . . ? 
O31 Si18 O45 108.7(4) . . ? 
O44 Si18 O45 110.6(3) . . ? 
O31 Si18 O32 109.1(3) . . ? 
O44 Si18 O32 111.5(4) . . ? 
O45 Si18 O32 109.6(4) . . ? 
O23 Si19 O33 110.3(3) . . ? 
O23 Si19 O22 110.5(3) . 2_646 ? 
O33 Si19 O22 107.9(4) . 2_646 ? 
O23 Si19 O43 107.2(3) . . ? 
O33 Si19 O43 110.3(4) . . ? 
O22 Si19 O43 110.7(4) 2_646 . ? 
O34 Si20 O39 110.4(3) . . ? 
O34 Si20 O33 108.7(3) . . ? 
O39 Si20 O33 110.2(4) . . ? 
O34 Si20 O38 109.0(3) . . ? 
O39 Si20 O38 108.9(4) . . ? 
O33 Si20 O38 109.6(4) . . ? 
O18 Si21 O35 109.6(4) 4_675 . ? 
O18 Si21 O34 109.5(3) 4_675 . ? 
O35 Si21 O34 108.7(3) . . ? 
O18 Si21 O25 107.7(3) 4_675 . ? 
O35 Si21 O25 110.4(3) . . ? 
O34 Si21 O25 111.0(3) . . ? 
O36 Si22 O15 109.6(4) . 4_675 ? 
O36 Si22 O26 110.7(3) . . ? 
O15 Si22 O26 108.6(3) 4_675 . ? 
O36 Si22 O35 108.2(4) . . ? 
O15 Si22 O35 109.2(3) 4_675 . ? 
O26 Si22 O35 110.5(3) . . ? 
O36 Si23 O40 109.1(4) . . ? 
O36 Si23 O37 110.9(4) . . ? 
O40 Si23 O37 109.1(4) . . ? 
O36 Si23 O48 109.1(4) . . ? 
O40 Si23 O48 110.4(3) . . ? 
O37 Si23 O48 108.3(4) . . ? 
O37 Si24 O38 110.1(4) . . ? 
O37 Si24 O24 109.2(3) . . ? 
O38 Si24 O24 107.7(3) . . ? 
O37 Si24 O46 110.5(4) . 4_575 ? 
O38 Si24 O46 111.7(4) . 4_575 ? 
O24 Si24 O46 107.6(3) . 4_575 ? 
Si1 O1 Si2 150.4(5) . . ? 
Si2 O2 Si3 149.3(4) . . ? 
Si4 O3 Si3 167.0(5) . . ? 
Si4 O4 Si5 151.3(5) . . ? 
Si6 O5 Si5 147.6(4) . . ? 
Si2 O6 Si6 163.1(5) . . ? 
Si8 O7 Si7 156.7(5) . . ? 
Si9 O8 Si8 153.8(4) . . ? 
Si10 O9 Si9 151.5(4) . . ? 
Si11 O10 Si10 158.5(5) . . ? 
Si11 O11 Si12 155.6(5) . . ? 
Si8 O12 Si12 172.1(5) . . ? 
Si8 O13 Si2 167.7(5) . . ? 
Si11 O14 Si5 164.1(4) . . ? 
Si1 O15 Si22 150.6(5) . 4_576 ? 
Si16 O16 Si1 178.6(5) . . ? 
Si7 O17 Si16 147.8(4) . . ? 
Si21 O18 Si6 143.9(4) 4_576 . ? 
Si15 O19 Si6 166.6(5) 4_576 . ? 
Si15 O20 Si12 145.9(4) 4_576 . ? 
Si13 O21 Si5 146.1(4) 2_656 . ? 
Si11 O22 Si19 150.8(5) . 2_656 ? 
Si19 O23 Si7 154.5(3) . . ? 
Si12 O24 Si24 149.5(3) . . ? 
Si9 O25 Si21 151.9(3) . . ? 
Si22 O26 Si10 145.6(3) . . ? 
Si14 O27 Si13 152.2(5) . . ? 
Si15 O28 Si14 150.9(4) . . ? 
Si15 O29 Si16 167.8(5) . 4_675 ? 
Si16 O30 Si17 158.1(5) 4_675 . ? 
Si18 O31 Si17 150.0(4) . . ? 
Si14 O32 Si18 159.2(5) . . ? 
Si19 O33 Si20 153.2(5) . . ? 
Si20 O34 Si21 150.3(4) . . ? 
Si21 O35 Si22 152.1(4) . . ? 
Si23 O36 Si22 163.6(5) . . ? 
Si24 O37 Si23 153.3(5) . . ? 
Si24 O38 Si20 157.6(5) . . ? 
Si20 O39 Si14 169.4(5) . . ? 
Si17 O40 Si23 165.1(4) . . ? 
Si10 O41 Si13 148.4(4) 4_575 . ? 
Si4 O42 Si13 161.2(5) 4_575 . ? 
Si4 O43 Si19 149.5(4) 4_575 . ? 
Si18 O44 Si9 148.5(4) . 4_575 ? 
Si18 O45 Si3 157.0(5) . 4_575 ? 
Si3 O46 Si24 152.0(5) . 4_676 ? 
Si17 O47 Si1 149.2(4) . 2_656 ? 
Si7 O48 Si23 149.2(5) 2_656 . ? 
  
_diffrn_measured_fraction_theta_max    0.948 
_diffrn_reflns_theta_full              28.71 
_diffrn_measured_fraction_theta_full   0.948 
_refine_diff_density_max    0.538 
_refine_diff_density_min   -0.499 
_refine_diff_density_rms    0.117 




  
data_f_2butyne_7d_mo 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C7.1 H0 O48 Si24' 
_chemical_formula_weight          1528 
  
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' 
 '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' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    13.33(3) 
_cell_length_b                    20.04(4) 
_cell_length_c                    19.81(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  89.97(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      5292(19) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.16 
_exptl_crystal_size_mid           0.09 
_exptl_crystal_size_min           0.05 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.878 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3000 
_exptl_absorpt_coefficient_mu     0.684 
_exptl_absorpt_correction_type    Analytical 
_exptl_absorpt_correction_T_min   0.8990 
_exptl_absorpt_correction_T_max   0.9653 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       296(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   'Bruker P4' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             62211 
_diffrn_reflns_av_R_equivalents   0.1316 
_diffrn_reflns_av_sigmaI/netI     0.1521 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -25 
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        -26 
_diffrn_reflns_limit_l_max        26 
_diffrn_reflns_theta_min          1.02 
_diffrn_reflns_theta_max          28.70 
_reflns_number_total              12818 
_reflns_number_gt                 5423 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker XSCANS' 
_computing_cell_refinement        'Bruker XSCANS' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_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)+(0.0467P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none 
_refine_ls_hydrogen_treatment     none 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          12818 
_refine_ls_number_parameters      676 
_refine_ls_number_restraints      15 
_refine_ls_R_factor_all           0.1506 
_refine_ls_R_factor_gt            0.0550 
_refine_ls_wR_factor_ref          0.1353 
_refine_ls_wR_factor_gt           0.1114 
_refine_ls_goodness_of_fit_ref    0.835 
_refine_ls_restrained_S_all       0.840 
_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 
C101 C 0.492(2) 1.0010(16) 0.0075(12) 0.27(2) Uiso 0.483(16) 1 d PGU . 1 
C102 C 0.4964(16) 0.9987(11) 0.0811(12) 0.143(16) Uiso 0.483(16) 1 d PGU . 1 
C103 C 0.5002(12) 0.9969(8) 0.1421(12) 0.19(2) Uiso 0.483(16) 1 d PGU . 1 
C104 C 0.5047(9) 0.9946(6) 0.2157(12) 0.152(18) Uiso 0.483(16) 1 d PGU . 1 
C201 C 0.492(3) 1.0014(19) 0.5145(12) 0.098(17) Uiso 0.326(13) 1 d PGU . 2 
C202 C 0.504(2) 1.0026(15) 0.4413(12) 0.087(15) Uiso 0.326(13) 1 d PGU . 2 
C203 C 0.5137(18) 1.0036(11) 0.3806(12) 0.14(2) Uiso 0.326(13) 1 d PGU . 2 
C204 C 0.5258(12) 1.0048(7) 0.3073(12) 0.17(3) Uiso 0.326(13) 1 d PGU . 2 
C301 C 0.8452(11) 0.8262(10) 0.2588(13) 0.41(3) Uiso 0.655(12) 1 d PGU A 3 
C302 C 0.8552(15) 0.7537(11) 0.2553(15) 0.45(3) Uiso 0.655(12) 1 d PGU A 3 
C303 C 0.8635(18) 0.6936(11) 0.2524(17) 0.86(6) Uiso 0.655(12) 1 d PGU A 3 
C304 C 0.874(2) 0.6212(11) 0.249(2) 0.70(5) Uiso 0.655(12) 1 d PGU A 3 
C401 C 0.8646(9) 0.8963(11) 0.2590(13) 0.19(3) Uiso 0.319(10) 1 d PGU B 4 
C402 C 0.7820(9) 0.9439(9) 0.2540(12) 0.31(4) Uiso 0.319(10) 1 d PGU B 4 
C403 C 0.7136(9) 0.9834(8) 0.2499(12) 0.38(5) Uiso 0.319(10) 1 d PGU B 4 
C404 C 0.6311(10) 1.0310(6) 0.2449(12) 0.25(3) Uiso 0.319(10) 1 d PGU B 4 
Si1 Si 0.32485(19) 0.42056(11) -0.05600(14) 0.0136(5) Uani 1 1 d . . . 
Si2 Si 0.1716(2) 0.31138(13) -0.03060(11) 0.0154(5) Uani 1 1 d . . . 
Si3 Si -0.04686(19) 0.27943(12) -0.06217(14) 0.0153(5) Uani 1 1 d . . . 
Si4 Si -0.03400(18) 0.12354(12) -0.06288(13) 0.0137(6) Uani 1 1 d . . . 
Si5 Si 0.1786(2) 0.07568(11) -0.02814(12) 0.0127(6) Uani 1 1 d . . . 
Si6 Si 0.31864(19) 0.19289(12) -0.05617(13) 0.0153(5) Uani 1 1 d . . . 
Si7 Si 0.3221(2) 0.42445(12) 0.17163(13) 0.0128(6) Uani 1 1 d . . . 
Si8 Si 0.17752(19) 0.31054(13) 0.12708(12) 0.0149(5) Uani 1 1 d . . . 
Si9 Si -0.03354(19) 0.27341(12) 0.17539(12) 0.0140(6) Uani 1 1 d . . . 
Si10 Si -0.0307(2) 0.11963(12) 0.17577(12) 0.0142(6) Uani 1 1 d . . . 
Si11 Si 0.1793(2) 0.07107(11) 0.12943(13) 0.0145(6) Uani 1 1 d . . . 
Si12 Si 0.3170(2) 0.18931(13) 0.16696(12) 0.0143(5) Uani 1 1 d . . . 
Si13 Si 0.33617(19) 0.42725(11) 0.55780(15) 0.0138(5) Uani 1 1 d . . . 
Si14 Si 0.1903(2) 0.31129(13) 0.52765(11) 0.0158(6) Uani 1 1 d . . . 
Si15 Si -0.02812(18) 0.27795(12) 0.56124(14) 0.0143(5) Uani 1 1 d . . . 
Si16 Si -0.03152(18) 0.12188(12) 0.56379(14) 0.0140(6) Uani 1 1 d . . . 
Si17 Si 0.1816(2) 0.07053(12) 0.52748(12) 0.0134(6) Uani 1 1 d . . . 
Si18 Si 0.32137(19) 0.18654(11) 0.56235(13) 0.0137(5) Uani 1 1 d . . . 
Si19 Si 0.3182(2) 0.42375(12) 0.32777(13) 0.0148(6) Uani 1 1 d . . . 
Si20 Si 0.17482(19) 0.31107(13) 0.36949(13) 0.0148(5) Uani 1 1 d . . . 
Si21 Si -0.0407(2) 0.27370(12) 0.33081(12) 0.0143(6) Uani 1 1 d . . . 
Si22 Si -0.0355(2) 0.11899(13) 0.32952(13) 0.0153(6) Uani 1 1 d . . . 
Si23 Si 0.1790(2) 0.07156(11) 0.36936(13) 0.0133(5) Uani 1 1 d . . . 
Si24 Si 0.30449(19) 0.19174(13) 0.32115(11) 0.0151(5) Uani 1 1 d . . . 
O1 O 0.2272(5) 0.3756(3) -0.0582(4) 0.0307(16) Uani 1 1 d . . . 
O2 O 0.0634(4) 0.3083(3) -0.0646(3) 0.0241(14) Uani 1 1 d . . . 
O3 O -0.0438(5) 0.2018(3) -0.0507(3) 0.0403(17) Uani 1 1 d . . . 
O4 O 0.0818(4) 0.1035(3) -0.0657(3) 0.0230(15) Uani 1 1 d . . . 
O5 O 0.2728(4) 0.1201(3) -0.0467(3) 0.0247(16) Uani 1 1 d . . . 
O6 O 0.2303(5) 0.2456(3) -0.0481(4) 0.0349(17) Uani 1 1 d . . . 
O7 O 0.2318(5) 0.3749(3) 0.1549(3) 0.033(2) Uani 1 1 d . . . 
O8 O 0.0730(5) 0.3048(3) 0.1642(3) 0.0309(16) Uani 1 1 d . . . 
O9 O -0.0304(5) 0.1963(3) 0.1553(3) 0.0270(17) Uani 1 1 d . . . 
O10 O 0.0780(5) 0.0898(3) 0.1673(3) 0.0312(17) Uani 1 1 d . . . 
O11 O 0.2680(5) 0.1197(3) 0.1518(3) 0.0265(17) Uani 1 1 d . . . 
O12 O 0.2443(5) 0.2464(3) 0.1402(3) 0.0364(18) Uani 1 1 d . . . 
O13 O 0.1601(5) 0.3172(3) 0.0489(3) 0.0444(19) Uani 1 1 d . . . 
O14 O 0.1598(4) 0.0778(3) 0.0505(3) 0.0281(15) Uani 1 1 d . . . 
O15 O 0.3808(5) 0.4147(3) -0.1257(3) 0.0296(18) Uani 1 1 d . . . 
O16 O 0.3959(6) 0.3969(4) 0.0034(3) 0.044(2) Uani 1 1 d . . . 
O17 O 0.4198(5) 0.4013(3) 0.1336(3) 0.0272(17) Uani 1 1 d . . . 
O18 O 0.3656(4) 0.1987(3) -0.1294(3) 0.0249(15) Uani 1 1 d . . . 
O19 O 0.4042(5) 0.2054(3) -0.0026(3) 0.0331(17) Uani 1 1 d . . . 
O20 O 0.4206(4) 0.1954(3) 0.1282(3) 0.0273(15) Uani 1 1 d . . . 
O21 O 0.2029(4) 0.0017(2) -0.0523(3) 0.0211(14) Uani 1 1 d . . . 
O22 O 0.2094(5) -0.0032(3) 0.1484(3) 0.0279(18) Uani 1 1 d . . . 
O23 O 0.3458(3) 0.4233(2) 0.2504(4) 0.0289(12) Uani 1 1 d . . . 
O24 O 0.3410(3) 0.1966(2) 0.2460(3) 0.0274(12) Uani 1 1 d . . . 
O25 O -0.0625(3) 0.2828(2) 0.2527(3) 0.0230(12) Uani 1 1 d . . . 
O26 O -0.0658(3) 0.1103(2) 0.2526(3) 0.0196(11) Uani 1 1 d . . . 
O27 O 0.2443(5) 0.3765(3) 0.5530(4) 0.0348(18) Uani 1 1 d . . . 
O28 O 0.0775(4) 0.3129(3) 0.5543(3) 0.0249(14) Uani 1 1 d . . . 
O29 O -0.0132(5) 0.2002(3) 0.5658(3) 0.0363(17) Uani 1 1 d . . . 
O30 O 0.0709(4) 0.0842(3) 0.5544(4) 0.0291(15) Uani 1 1 d . . . 
O31 O 0.2598(5) 0.1197(3) 0.5641(3) 0.0251(16) Uani 1 1 d . . . 
O32 O 0.2470(5) 0.2486(3) 0.5593(3) 0.0308(16) Uani 1 1 d . . . 
O33 O 0.2244(5) 0.3778(3) 0.3416(3) 0.0294(18) Uani 1 1 d . . . 
O34 O 0.0588(4) 0.3132(3) 0.3541(3) 0.0238(15) Uani 1 1 d . . . 
O35 O -0.0251(5) 0.1964(3) 0.3482(3) 0.0263(17) Uani 1 1 d . . . 
O36 O 0.0694(5) 0.0840(3) 0.3429(3) 0.038(2) Uani 1 1 d . . . 
O37 O 0.2560(6) 0.1201(3) 0.3339(3) 0.0335(19) Uani 1 1 d . . . 
O38 O 0.2228(5) 0.2476(3) 0.3340(3) 0.0315(17) Uani 1 1 d . . . 
O39 O 0.1941(5) 0.3060(4) 0.4489(3) 0.0453(17) Uani 1 1 d . . . 
O40 O 0.1833(5) 0.0837(3) 0.4484(3) 0.0346(16) Uani 1 1 d . . . 
O41 O 0.3924(5) 0.4192(3) 0.6286(3) 0.0312(18) Uani 1 1 d . . . 
O42 O 0.4126(5) 0.4132(3) 0.4984(3) 0.0293(16) Uani 1 1 d . . . 
O43 O 0.4144(5) 0.3973(3) 0.3683(3) 0.0274(17) Uani 1 1 d . . . 
O44 O 0.3855(4) 0.1891(3) 0.6296(3) 0.0242(15) Uani 1 1 d . . . 
O45 O 0.3935(5) 0.1867(3) 0.4980(3) 0.0305(17) Uani 1 1 d . . . 
O46 O -0.0998(5) 0.2962(4) -0.1311(3) 0.0365(18) Uani 1 1 d . . . 
O47 O 0.2092(5) -0.0042(3) 0.5442(3) 0.0227(16) Uani 1 1 d . . . 
O48 O 0.2109(5) -0.0027(3) 0.3516(3) 0.0268(17) Uani 1 1 d . . . 
  
  
_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 
C101 C101 0.37(6) 3_675 ? 
C101 C102 1.4600 . ? 
C101 C102 1.76(5) 3_675 ? 
C102 C103 1.2100 . ? 
C102 C101 1.76(5) 3_675 ? 
C103 C104 1.4600 . ? 
C201 C201 0.62(4) 3_676 ? 
C201 C202 0.88(5) 3_676 ? 
C201 C202 1.4599 . ? 
C202 C201 0.88(5) 3_676 ? 
C202 C203 1.2099 . ? 
C203 C204 1.4599 . ? 
C301 C302 1.4600 . ? 
C302 C303 1.2100 . ? 
C303 C304 1.4600 . ? 
C401 C402 1.4600 . ? 
C402 C403 1.2101 . ? 
C403 C404 1.4600 . ? 
Si1 O15 1.573(7) . ? 
Si1 O16 1.584(7) . ? 
Si1 O1 1.584(7) . ? 
Si1 O47 1.592(7) 2 ? 
Si2 O6 1.572(7) . ? 
Si2 O1 1.582(7) . ? 
Si2 O13 1.586(7) . ? 
Si2 O2 1.594(6) . ? 
Si3 O3 1.573(7) . ? 
Si3 O46 1.575(7) . ? 
Si3 O2 1.580(7) . ? 
Si3 O45 1.585(7) 4_565 ? 
Si4 O43 1.583(7) 4_565 ? 
Si4 O42 1.587(7) 4_565 ? 
Si4 O3 1.592(7) . ? 
Si4 O4 1.596(7) . ? 
Si5 O14 1.579(8) . ? 
Si5 O5 1.582(7) . ? 
Si5 O4 1.591(6) . ? 
Si5 O21 1.592(6) . ? 
Si6 O19 1.579(7) . ? 
Si6 O18 1.584(7) . ? 
Si6 O6 1.590(7) . ? 
Si6 O5 1.593(6) . ? 
Si7 O17 1.574(7) . ? 
Si7 O48 1.592(7) 2 ? 
Si7 O23 1.593(8) . ? 
Si7 O7 1.596(7) . ? 
Si8 O13 1.572(7) . ? 
Si8 O7 1.578(7) . ? 
Si8 O8 1.580(7) . ? 
Si8 O12 1.585(7) . ? 
Si9 O8 1.568(7) . ? 
Si9 O25 1.590(7) . ? 
Si9 O9 1.597(7) . ? 
Si9 O44 1.598(7) 4_565 ? 
Si10 O10 1.576(7) . ? 
Si10 O9 1.588(7) . ? 
Si10 O41 1.590(7) 4_565 ? 
Si10 O26 1.603(7) . ? 
Si11 O22 1.586(7) . ? 
Si11 O10 1.589(7) . ? 
Si11 O14 1.590(8) . ? 
Si11 O11 1.596(7) . ? 
Si12 O11 1.570(7) . ? 
Si12 O20 1.583(7) . ? 
Si12 O12 1.591(7) . ? 
Si12 O24 1.605(7) . ? 
Si13 O42 1.582(7) . ? 
Si13 O21 1.583(6) 2 ? 
Si13 O27 1.595(7) . ? 
Si13 O41 1.599(7) . ? 
Si14 O39 1.565(7) . ? 
Si14 O27 1.574(7) . ? 
Si14 O28 1.593(7) . ? 
Si14 O32 1.595(6) . ? 
Si15 O29 1.573(7) . ? 
Si15 O28 1.578(6) . ? 
Si15 O20 1.586(7) 4_566 ? 
Si15 O19 1.589(7) 4_566 ? 
Si16 O30 1.572(6) . ? 
Si16 O16 1.584(7) 4_566 ? 
Si16 O29 1.589(7) . ? 
Si16 O17 1.597(7) 4_566 ? 
Si17 O47 1.578(7) . ? 
Si17 O40 1.589(7) . ? 
Si17 O30 1.591(7) . ? 
Si17 O31 1.608(6) . ? 
Si18 O31 1.572(6) . ? 
Si18 O44 1.584(7) . ? 
Si18 O32 1.592(6) . ? 
Si18 O45 1.596(7) . ? 
Si19 O23 1.576(8) . ? 
Si19 O33 1.576(7) . ? 
Si19 O22 1.582(7) 2 ? 
Si19 O43 1.604(7) . ? 
Si20 O34 1.577(7) . ? 
Si20 O38 1.587(6) . ? 
Si20 O33 1.590(7) . ? 
Si20 O39 1.597(7) . ? 
Si21 O18 1.577(6) 4_566 ? 
Si21 O25 1.586(7) . ? 
Si21 O35 1.600(7) . ? 
Si21 O34 1.612(7) . ? 
Si22 O15 1.578(7) 4_566 ? 
Si22 O26 1.586(8) . ? 
Si22 O36 1.587(8) . ? 
Si22 O35 1.601(7) . ? 
Si23 O36 1.571(8) . ? 
Si23 O37 1.579(7) . ? 
Si23 O40 1.585(7) . ? 
Si23 O48 1.587(7) . ? 
Si24 O24 1.569(7) . ? 
Si24 O38 1.582(7) . ? 
Si24 O37 1.595(7) . ? 
Si24 O46 1.606(7) 4_666 ? 
O15 Si22 1.578(7) 4_665 ? 
O16 Si16 1.584(7) 4_665 ? 
O17 Si16 1.597(7) 4_665 ? 
O18 Si21 1.577(6) 4_665 ? 
O19 Si15 1.589(7) 4_665 ? 
O20 Si15 1.586(7) 4_665 ? 
O21 Si13 1.583(6) 2_545 ? 
O22 Si19 1.582(7) 2_545 ? 
O41 Si10 1.590(7) 4_666 ? 
O42 Si4 1.587(7) 4_666 ? 
O43 Si4 1.583(7) 4_666 ? 
O44 Si9 1.598(7) 4_666 ? 
O45 Si3 1.585(7) 4_666 ? 
O46 Si24 1.606(7) 4_565 ? 
O47 Si1 1.592(7) 2_545 ? 
O48 Si7 1.592(7) 2_545 ? 
  
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 
C101 C101 C102 141(7) 3_675 . ? 
C101 C101 C102 32(5) 3_675 3_675 ? 
C102 C101 C102 172(2) . 3_675 ? 
C103 C102 C101 180.0 . . ? 
C103 C102 C101 172.3(18) . 3_675 ? 
C101 C102 C101 7.7(18) . 3_675 ? 
C102 C103 C104 180.0 . . ? 
C201 C201 C202 153(10) 3_676 3_676 ? 
C201 C201 C202 16(6) 3_676 . ? 
C202 C201 C202 169(5) 3_676 . ? 
C201 C202 C203 169(4) 3_676 . ? 
C201 C202 C201 11(4) 3_676 . ? 
C203 C202 C201 180(5) . . ? 
C202 C203 C204 180(4) . . ? 
C303 C302 C301 180.0 . . ? 
C302 C303 C304 180.0 . . ? 
C403 C402 C401 180.0 . . ? 
C402 C403 C404 180.0(12) . . ? 
O15 Si1 O16 110.3(4) . . ? 
O15 Si1 O1 108.8(4) . . ? 
O16 Si1 O1 110.0(4) . . ? 
O15 Si1 O47 109.5(4) . 2 ? 
O16 Si1 O47 110.2(4) . 2 ? 
O1 Si1 O47 108.0(4) . 2 ? 
O6 Si2 O1 111.9(4) . . ? 
O6 Si2 O13 109.2(4) . . ? 
O1 Si2 O13 109.2(4) . . ? 
O6 Si2 O2 108.9(4) . . ? 
O1 Si2 O2 108.0(4) . . ? 
O13 Si2 O2 109.7(4) . . ? 
O3 Si3 O46 110.4(4) . . ? 
O3 Si3 O2 110.0(4) . . ? 
O46 Si3 O2 108.2(4) . . ? 
O3 Si3 O45 109.2(4) . 4_565 ? 
O46 Si3 O45 109.7(4) . 4_565 ? 
O2 Si3 O45 109.4(4) . 4_565 ? 
O43 Si4 O42 109.9(4) 4_565 4_565 ? 
O43 Si4 O3 110.8(4) 4_565 . ? 
O42 Si4 O3 107.7(4) 4_565 . ? 
O43 Si4 O4 108.9(4) 4_565 . ? 
O42 Si4 O4 110.1(4) 4_565 . ? 
O3 Si4 O4 109.4(3) . . ? 
O14 Si5 O5 109.8(4) . . ? 
O14 Si5 O4 108.9(4) . . ? 
O5 Si5 O4 109.8(4) . . ? 
O14 Si5 O21 110.7(3) . . ? 
O5 Si5 O21 107.0(4) . . ? 
O4 Si5 O21 110.5(4) . . ? 
O19 Si6 O18 108.6(4) . . ? 
O19 Si6 O6 111.3(4) . . ? 
O18 Si6 O6 109.6(4) . . ? 
O19 Si6 O5 110.1(4) . . ? 
O18 Si6 O5 109.0(4) . . ? 
O6 Si6 O5 108.2(4) . . ? 
O17 Si7 O48 111.1(4) . 2 ? 
O17 Si7 O23 107.4(4) . . ? 
O48 Si7 O23 110.6(3) 2 . ? 
O17 Si7 O7 109.9(4) . . ? 
O48 Si7 O7 107.6(4) 2 . ? 
O23 Si7 O7 110.2(3) . . ? 
O13 Si8 O7 110.0(4) . . ? 
O13 Si8 O8 109.6(4) . . ? 
O7 Si8 O8 107.5(4) . . ? 
O13 Si8 O12 108.3(4) . . ? 
O7 Si8 O12 110.4(4) . . ? 
O8 Si8 O12 111.1(4) . . ? 
O8 Si9 O25 107.9(3) . . ? 
O8 Si9 O9 109.2(4) . . ? 
O25 Si9 O9 111.1(3) . . ? 
O8 Si9 O44 110.0(4) . 4_565 ? 
O25 Si9 O44 109.1(3) . 4_565 ? 
O9 Si9 O44 109.4(4) . 4_565 ? 
O10 Si10 O9 109.7(4) . . ? 
O10 Si10 O41 110.1(4) . 4_565 ? 
O9 Si10 O41 108.9(4) . 4_565 ? 
O10 Si10 O26 108.9(3) . . ? 
O9 Si10 O26 110.8(3) . . ? 
O41 Si10 O26 108.2(4) 4_565 . ? 
O22 Si11 O10 108.9(4) . . ? 
O22 Si11 O14 110.7(4) . . ? 
O10 Si11 O14 107.8(4) . . ? 
O22 Si11 O11 108.6(4) . . ? 
O10 Si11 O11 110.8(4) . . ? 
O14 Si11 O11 110.1(4) . . ? 
O11 Si12 O20 109.8(4) . . ? 
O11 Si12 O12 108.8(4) . . ? 
O20 Si12 O12 108.3(4) . . ? 
O11 Si12 O24 110.5(3) . . ? 
O20 Si12 O24 106.9(3) . . ? 
O12 Si12 O24 112.4(3) . . ? 
O42 Si13 O21 109.2(4) . 2 ? 
O42 Si13 O27 109.6(4) . . ? 
O21 Si13 O27 110.1(4) 2 . ? 
O42 Si13 O41 109.4(4) . . ? 
O21 Si13 O41 108.1(4) 2 . ? 
O27 Si13 O41 110.4(4) . . ? 
O39 Si14 O27 111.1(4) . . ? 
O39 Si14 O28 111.2(4) . . ? 
O27 Si14 O28 108.0(4) . . ? 
O39 Si14 O32 108.9(4) . . ? 
O27 Si14 O32 108.1(4) . . ? 
O28 Si14 O32 109.5(3) . . ? 
O29 Si15 O28 109.4(4) . . ? 
O29 Si15 O20 109.9(4) . 4_566 ? 
O28 Si15 O20 107.9(4) . 4_566 ? 
O29 Si15 O19 109.0(4) . 4_566 ? 
O28 Si15 O19 110.1(4) . 4_566 ? 
O20 Si15 O19 110.5(4) 4_566 4_566 ? 
O30 Si16 O16 109.1(4) . 4_566 ? 
O30 Si16 O29 110.2(3) . . ? 
O16 Si16 O29 110.4(4) 4_566 . ? 
O30 Si16 O17 108.4(4) . 4_566 ? 
O16 Si16 O17 109.7(4) 4_566 4_566 ? 
O29 Si16 O17 109.1(4) . 4_566 ? 
O47 Si17 O40 111.2(3) . . ? 
O47 Si17 O30 108.0(3) . . ? 
O40 Si17 O30 108.4(4) . . ? 
O47 Si17 O31 109.6(4) . . ? 
O40 Si17 O31 109.5(4) . . ? 
O30 Si17 O31 110.1(4) . . ? 
O31 Si18 O44 106.9(4) . . ? 
O31 Si18 O32 110.0(4) . . ? 
O44 Si18 O32 110.1(4) . . ? 
O31 Si18 O45 109.6(4) . . ? 
O44 Si18 O45 110.2(4) . . ? 
O32 Si18 O45 110.1(4) . . ? 
O23 Si19 O33 110.5(3) . . ? 
O23 Si19 O22 110.5(3) . 2 ? 
O33 Si19 O22 107.8(4) . 2 ? 
O23 Si19 O43 107.4(4) . . ? 
O33 Si19 O43 110.7(4) . . ? 
O22 Si19 O43 110.0(4) 2 . ? 
O34 Si20 O38 109.3(4) . . ? 
O34 Si20 O33 108.5(4) . . ? 
O38 Si20 O33 110.7(4) . . ? 
O34 Si20 O39 110.5(3) . . ? 
O38 Si20 O39 108.6(4) . . ? 
O33 Si20 O39 109.2(4) . . ? 
O18 Si21 O25 107.6(3) 4_566 . ? 
O18 Si21 O35 109.6(4) 4_566 . ? 
O25 Si21 O35 110.2(3) . . ? 
O18 Si21 O34 109.6(3) 4_566 . ? 
O25 Si21 O34 111.9(3) . . ? 
O35 Si21 O34 107.9(4) . . ? 
O15 Si22 O26 108.2(3) 4_566 . ? 
O15 Si22 O36 109.9(4) 4_566 . ? 
O26 Si22 O36 109.7(3) . . ? 
O15 Si22 O35 110.3(4) 4_566 . ? 
O26 Si22 O35 110.5(3) . . ? 
O36 Si22 O35 108.3(4) . . ? 
O36 Si23 O37 111.0(4) . . ? 
O36 Si23 O40 109.8(4) . . ? 
O37 Si23 O40 108.7(4) . . ? 
O36 Si23 O48 108.9(4) . . ? 
O37 Si23 O48 107.7(4) . . ? 
O40 Si23 O48 110.7(4) . . ? 
O24 Si24 O38 108.8(3) . . ? 
O24 Si24 O37 109.4(3) . . ? 
O38 Si24 O37 109.4(4) . . ? 
O24 Si24 O46 107.6(4) . 4_666 ? 
O38 Si24 O46 110.2(4) . 4_666 ? 
O37 Si24 O46 111.4(4) . 4_666 ? 
Si2 O1 Si1 146.9(5) . . ? 
Si3 O2 Si2 147.5(4) . . ? 
Si3 O3 Si4 162.7(5) . . ? 
Si5 O4 Si4 148.9(4) . . ? 
Si5 O5 Si6 147.8(4) . . ? 
Si2 O6 Si6 161.4(5) . . ? 
Si8 O7 Si7 158.0(5) . . ? 
Si9 O8 Si8 153.3(5) . . ? 
Si10 O9 Si9 150.8(4) . . ? 
Si10 O10 Si11 156.9(5) . . ? 
Si12 O11 Si11 154.8(5) . . ? 
Si8 O12 Si12 168.6(5) . . ? 
Si8 O13 Si2 163.3(5) . . ? 
Si5 O14 Si11 160.4(4) . . ? 
Si1 O15 Si22 149.3(5) . 4_665 ? 
Si16 O16 Si1 176.4(5) 4_665 . ? 
Si7 O17 Si16 146.7(5) . 4_665 ? 
Si21 O18 Si6 142.7(4) 4_665 . ? 
Si6 O19 Si15 168.3(5) . 4_665 ? 
Si12 O20 Si15 143.8(4) . 4_665 ? 
Si13 O21 Si5 146.2(4) 2_545 . ? 
Si19 O22 Si11 151.7(5) 2_545 . ? 
Si19 O23 Si7 155.0(3) . . ? 
Si24 O24 Si12 149.1(3) . . ? 
Si21 O25 Si9 151.9(3) . . ? 
Si22 O26 Si10 145.6(3) . . ? 
Si14 O27 Si13 154.2(5) . . ? 
Si15 O28 Si14 149.5(4) . . ? 
Si15 O29 Si16 163.2(5) . . ? 
Si16 O30 Si17 158.0(5) . . ? 
Si18 O31 Si17 148.3(5) . . ? 
Si18 O32 Si14 157.7(5) . . ? 
Si19 O33 Si20 151.7(5) . . ? 
Si20 O34 Si21 148.1(4) . . ? 
Si21 O35 Si22 151.3(4) . . ? 
Si23 O36 Si22 160.9(5) . . ? 
Si23 O37 Si24 152.7(5) . . ? 
Si24 O38 Si20 156.3(5) . . ? 
Si14 O39 Si20 166.5(5) . . ? 
Si23 O40 Si17 161.4(4) . . ? 
Si10 O41 Si13 150.2(5) 4_666 . ? 
Si13 O42 Si4 160.0(5) . 4_666 ? 
Si4 O43 Si19 150.1(5) 4_666 . ? 
Si18 O44 Si9 149.0(4) . 4_666 ? 
Si3 O45 Si18 154.6(5) 4_666 . ? 
Si3 O46 Si24 154.0(5) . 4_565 ? 
Si17 O47 Si1 149.7(5) . 2_545 ? 
Si23 O48 Si7 148.2(5) . 2_545 ? 
  
_diffrn_measured_fraction_theta_max    0.939 
_diffrn_reflns_theta_full              28.70 
_diffrn_measured_fraction_theta_full   0.939 
_refine_diff_density_max    0.686 
_refine_diff_density_min   -0.675 
_refine_diff_density_rms    0.148 




  
data_f_c2butene_twin_96h_uc 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C4.4 H0 O48 Si24' 
_chemical_formula_weight          1495
  
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' 
 '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' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    13.549(4) 
_cell_length_b                    20.223(6) 
_cell_length_c                    20.059(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.103(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      5496(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.16 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.06 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.811 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3008 
_exptl_absorpt_coefficient_mu     0.659 
_exptl_absorpt_correction_type    Analytical 
_exptl_absorpt_correction_T_min   0.9025 
_exptl_absorpt_correction_T_max   0.9634 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       296(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   'Bruker P4' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             65301 
_diffrn_reflns_av_R_equivalents   0.0845 
_diffrn_reflns_av_sigmaI/netI     0.1097 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        -27 
_diffrn_reflns_limit_k_max        27 
_diffrn_reflns_limit_l_min        -25 
_diffrn_reflns_limit_l_max        27 
_diffrn_reflns_theta_min          1.01 
_diffrn_reflns_theta_max          28.75 
_reflns_number_total              13365 
_reflns_number_gt                 5411 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker XSCANS' 
_computing_cell_refinement        'Bruker XSCANS' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_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)+(0.0668P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none
_refine_ls_hydrogen_treatment     none 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          13365 
_refine_ls_number_parameters      676 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1353 
_refine_ls_R_factor_gt            0.0486 
_refine_ls_wR_factor_ref          0.1682 
_refine_ls_wR_factor_gt           0.1409 
_refine_ls_goodness_of_fit_ref    0.887 
_refine_ls_restrained_S_all       0.887 
_refine_ls_shift/su_max           0.050 
_refine_ls_shift/su_mean          0.006 
  
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 
C301 C 0.1820(11) 0.2295(9) 0.7599(9) 0.18(3) Uiso 0.289(18) 1 d PG A 1 
C302 C 0.0911(10) 0.1911(10) 0.7407(10) 0.069(16) Uiso 0.289(18) 1 d PG A 1 
C303 C 0.0879(11) 0.1257(10) 0.7287(10) 0.21(4) Uiso 0.289(18) 1 d PG A 1 
C304 C 0.1747(12) 0.0793(9) 0.7323(10) 0.18(3) Uiso 0.289(18) 1 d PG A 1 
C501 C 0.1928(11) 0.2917(9) 0.7361(8) 0.109(14) Uiso 0.382(16) 1 d PG B 2 
C502 C 0.1042(10) 0.2467(9) 0.7349(9) 0.102(13) Uiso 0.382(16) 1 d PG B 2 
C503 C 0.1044(10) 0.1821(10) 0.7511(9) 0.19(3) Uiso 0.382(16) 1 d PG B 2 
C504 C 0.1933(11) 0.1434(9) 0.7734(9) 0.14(2) Uiso 0.382(16) 1 d PG B 2 
C101 C 0.561(2) 1.0149(11) -0.0411(12) 0.029(10) Uiso 0.230(9) 1 d PG . 3 
C102 C 0.480(2) 0.9752(11) -0.0095(12) 0.075(18) Uiso 0.230(9) 1 d PG . 3 
C103 C 0.4590(19) 0.9733(10) 0.0561(12) 0.031(10) Uiso 0.230(9) 1 d PG . 3 
C104 C 0.514(2) 1.0104(10) 0.1096(12) 0.084(18) Uiso 0.230(9) 1 d PG . 3 
C201 C 0.553(2) 0.0232(9) 0.5103(14) 0.057(17) Uiso 0.206(13) 1 d PG . 4 
C202 C 0.465(2) 0.0015(8) 0.4696(13) 0.19(6) Uiso 0.206(13) 1 d PG . 4 
C203 C 0.463(3) -0.0027(8) 0.4027(13) 0.09(2) Uiso 0.206(13) 1 d PG . 4 
C204 C 0.547(3) 0.0135(9) 0.3566(14) 0.28(7) Uiso 0.206(13) 1 d PG . 4 
Si1 Si 0.3401(3) 0.4224(2) -0.0575(3) 0.0173(12) Uani 1 1 d . . . 
Si2 Si 0.1946(4) 0.3063(3) -0.0297(2) 0.0172(12) Uani 1 1 d . . . 
Si3 Si -0.0281(3) 0.2792(2) -0.0617(3) 0.0180(11) Uani 1 1 d . . . 
Si4 Si -0.0253(3) 0.1226(2) -0.0632(2) 0.0163(11) Uani 1 1 d . . . 
Si5 Si 0.1871(4) 0.0712(2) -0.0285(2) 0.0155(12) Uani 1 1 d . . . 
Si6 Si 0.3336(3) 0.1841(3) -0.0594(3) 0.0192(11) Uani 1 1 d . . . 
Si7 Si 0.3283(4) 0.4225(3) 0.1720(2) 0.0182(12) Uani 1 1 d . . . 
Si8 Si 0.1899(4) 0.3064(2) 0.1289(2) 0.0178(11) Uani 1 1 d . . . 
Si9 Si -0.0264(4) 0.2754(2) 0.1726(2) 0.0176(12) Uani 1 1 d . . . 
Si10 Si -0.0250(4) 0.1203(3) 0.1742(2) 0.0171(11) Uani 1 1 d . . . 
Si11 Si 0.1864(4) 0.0696(2) 0.1302(2) 0.0161(12) Uani 1 1 d . . . 
Si12 Si 0.3227(4) 0.1853(3) 0.1726(2) 0.0182(11) Uani 1 1 d . . . 
Si13 Si 0.3395(3) 0.4229(2) 0.5576(3) 0.0151(11) Uani 1 1 d . . . 
Si14 Si 0.1939(4) 0.3063(3) 0.5292(2) 0.0188(12) Uani 1 1 d . . . 
Si15 Si -0.0270(3) 0.2807(2) 0.5617(2) 0.0169(11) Uani 1 1 d . . . 
Si16 Si -0.0240(3) 0.1229(2) 0.5642(2) 0.0163(11) Uani 1 1 d . . . 
Si17 Si 0.1880(3) 0.0711(2) 0.5285(2) 0.0146(12) Uani 1 1 d . . . 
Si18 Si 0.3322(3) 0.1843(2) 0.5597(3) 0.0166(11) Uani 1 1 d . . . 
Si19 Si 0.3279(4) 0.4226(2) 0.3278(2) 0.0162(11) Uani 1 1 d . . . 
Si20 Si 0.1886(4) 0.3064(3) 0.3710(2) 0.0178(11) Uani 1 1 d . . . 
Si21 Si -0.0280(4) 0.2746(2) 0.3282(2) 0.0175(12) Uani 1 1 d . . . 
Si22 Si -0.0259(4) 0.1203(3) 0.3276(2) 0.0186(12) Uani 1 1 d . . . 
Si23 Si 0.1849(4) 0.0699(2) 0.3706(2) 0.0166(12) Uani 1 1 d . . . 
Si24 Si 0.3233(3) 0.1851(3) 0.3268(2) 0.0161(11) Uani 1 1 d . . . 
O1 O 0.2520(8) 0.3711(6) -0.0551(8) 0.040(4) Uani 1 1 d . . . 
O2 O 0.0869(8) 0.3059(6) -0.0604(7) 0.029(3) Uani 1 1 d . . . 
O3 O -0.0287(11) 0.2007(6) -0.0625(7) 0.049(4) Uani 1 1 d . . . 
O4 O 0.0879(8) 0.0984(6) -0.0618(7) 0.034(4) Uani 1 1 d . . . 
O5 O 0.2814(8) 0.1129(6) -0.0552(7) 0.027(3) Uani 1 1 d . . . 
O6 O 0.2494(8) 0.2412(6) -0.0522(8) 0.045(4) Uani 1 1 d . . . 
O7 O 0.2437(10) 0.3706(7) 0.1558(8) 0.045(4) Uani 1 1 d . . . 
O8 O 0.0757(10) 0.3055(6) 0.1556(7) 0.041(4) Uani 1 1 d . . . 
O9 O -0.0244(12) 0.1988(6) 0.1544(6) 0.044(4) Uani 1 1 d . . . 
O10 O 0.0847(10) 0.0923(7) 0.1640(7) 0.043(4) Uani 1 1 d . . . 
O11 O 0.2809(8) 0.1143(6) 0.1562(6) 0.027(3) Uani 1 1 d . . . 
O12 O 0.2461(9) 0.2408(7) 0.1526(7) 0.047(4) Uani 1 1 d . . . 
O13 O 0.1944(11) 0.3075(8) 0.0499(8) 0.065(5) Uani 1 1 d . . . 
O14 O 0.1762(10) 0.0772(6) 0.0505(7) 0.039(4) Uani 1 1 d . . . 
O15 O 0.3996(10) 0.4182(7) -0.1276(6) 0.034(3) Uani 1 1 d . . . 
O16 O 0.4141(10) 0.4071(7) 0.0012(6) 0.043(4) Uani 1 1 d . . . 
O17 O 0.4278(9) 0.4015(7) 0.1326(6) 0.037(4) Uani 1 1 d . . . 
O18 O 0.3894(9) 0.1887(6) -0.1324(6) 0.025(3) Uani 1 1 d . . . 
O19 O 0.4141(10) 0.1898(6) -0.0015(6) 0.030(3) Uani 1 1 d . . . 
O20 O 0.4204(10) 0.1932(7) 0.1297(6) 0.037(4) Uani 1 1 d . . . 
O21 O 0.2035(8) -0.0049(5) -0.0508(7) 0.025(3) Uani 1 1 d . . . 
O22 O 0.2125(8) -0.0052(6) 0.1499(7) 0.029(3) Uani 1 1 d . . . 
O23 O 0.3533(3) 0.4227(2) 0.2528(8) 0.0364(13) Uani 1 1 d . . . 
O24 O 0.3528(3) 0.1897(2) 0.2526(8) 0.0304(12) Uani 1 1 d . . . 
O25 O -0.0503(3) 0.2849(2) 0.2482(7) 0.0316(12) Uani 1 1 d . . . 
O26 O -0.0574(3) 0.11097(18) 0.2489(7) 0.0244(10) Uani 1 1 d . . . 
O27 O 0.2493(9) 0.3697(6) 0.5569(8) 0.040(4) Uani 1 1 d . . . 
O28 O 0.0815(8) 0.3066(6) 0.5584(7) 0.034(3) Uani 1 1 d . . . 
O29 O -0.0327(10) 0.2015(6) 0.5554(7) 0.044(3) Uani 1 1 d . . . 
O30 O 0.0881(8) 0.0994(7) 0.5628(6) 0.032(3) Uani 1 1 d . . . 
O31 O 0.2800(8) 0.1135(6) 0.5542(7) 0.025(3) Uani 1 1 d . . . 
O32 O 0.2518(8) 0.2414(6) 0.5555(7) 0.040(4) Uani 1 1 d . . . 
O33 O 0.2389(9) 0.3712(6) 0.3414(7) 0.039(4) Uani 1 1 d . . . 
O34 O 0.0784(9) 0.3072(6) 0.3463(7) 0.037(4) Uani 1 1 d . . . 
O35 O -0.0263(11) 0.1962(5) 0.3477(5) 0.032(3) Uani 1 1 d . . . 
O36 O 0.0824(10) 0.0915(7) 0.3380(7) 0.043(4) Uani 1 1 d . . . 
O37 O 0.2680(9) 0.1156(7) 0.3409(7) 0.041(4) Uani 1 1 d . . . 
O38 O 0.2428(9) 0.2422(7) 0.3413(7) 0.047(4) Uani 1 1 d . . . 
O39 O 0.1891(11) 0.3069(8) 0.4501(7) 0.061(5) Uani 1 1 d . . . 
O40 O 0.1782(10) 0.0787(6) 0.4490(7) 0.035(3) Uani 1 1 d . . . 
O41 O 0.3929(10) 0.4186(7) 0.6268(6) 0.038(4) Uani 1 1 d . . . 
O42 O 0.4194(10) 0.4098(6) 0.4980(6) 0.032(3) Uani 1 1 d . . . 
O43 O 0.4266(8) 0.4019(7) 0.3681(6) 0.030(3) Uani 1 1 d . . . 
O44 O 0.3848(9) 0.1891(7) 0.6281(6) 0.033(3) Uani 1 1 d . . . 
O45 O 0.4121(11) 0.1932(7) 0.5006(6) 0.044(4) Uani 1 1 d . . . 
O46 O -0.0759(9) 0.3042(7) -0.1292(6) 0.035(4) Uani 1 1 d . . . 
O47 O 0.2068(8) -0.0038(5) 0.5480(7) 0.025(3) Uani 1 1 d . . . 
O48 O 0.2047(9) -0.0069(6) 0.3528(7) 0.033(3) Uani 1 1 d . . . 
  
  
_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 
C301 C302 1.5053 . ? 
C302 C303 1.3460 . ? 
C303 C304 1.5062 . ? 
C501 C502 1.5059 . ? 
C502 C503 1.3461 . ? 
C503 C504 1.5045 . ? 
C101 C103 0.47(4) 3_675 ? 
C101 C102 1.18(5) 3_675 ? 
C101 C102 1.5072 . ? 
C101 C104 1.78(6) 3_675 ? 
C102 C101 1.18(5) 3_675 ? 
C102 C102 1.21(5) 3_675 ? 
C102 C103 1.3465 . ? 
C102 C103 1.63(4) 3_675 ? 
C102 C104 2.03(4) 3_675 ? 
C103 C101 0.47(4) 3_675 ? 
C103 C104 1.5051 . ? 
C103 C102 1.63(4) 3_675 ? 
C104 C101 1.78(5) 3_675 ? 
C104 C102 2.03(5) 3_675 ? 
C201 C202 0.69(3) 3_656 ? 
C201 C202 1.5049 . ? 
C201 C201 1.76(7) 3_656 ? 
C201 C203 1.81(5) 3_656 ? 
C202 C201 0.69(4) 3_656 ? 
C202 C203 1.3460 . ? 
C202 C202 1.54(7) 3_656 ? 
C203 C204 1.5073 . ? 
C203 C201 1.81(5) 3_656 ? 
Si1 O16 1.575(13) . ? 
Si1 O1 1.583(12) . ? 
Si1 O15 1.625(13) . ? 
Si1 O47 1.633(12) 2 ? 
Si2 O6 1.578(13) . ? 
Si2 O2 1.583(12) . ? 
Si2 O13 1.596(15) . ? 
Si2 O1 1.607(13) . ? 
Si3 O46 1.581(12) . ? 
Si3 O3 1.588(12) . ? 
Si3 O45 1.592(13) 4_565 ? 
Si3 O2 1.649(12) . ? 
Si4 O42 1.581(12) 4_565 ? 
Si4 O3 1.582(12) . ? 
Si4 O43 1.602(12) 4_565 ? 
Si4 O4 1.609(12) . ? 
Si5 O14 1.595(13) . ? 
Si5 O4 1.598(12) . ? 
Si5 O21 1.618(12) . ? 
Si5 O5 1.622(12) . ? 
Si6 O19 1.595(12) . ? 
Si6 O5 1.607(12) . ? 
Si6 O6 1.629(12) . ? 
Si6 O18 1.652(12) . ? 
Si7 O48 1.577(13) 2 ? 
Si7 O7 1.588(13) . ? 
Si7 O17 1.620(13) . ? 
Si7 O23 1.656(16) . ? 
Si8 O7 1.583(14) . ? 
Si8 O13 1.586(15) . ? 
Si8 O12 1.602(14) . ? 
Si8 O8 1.638(14) . ? 
Si9 O8 1.550(13) . ? 
Si9 O25 1.561(14) . ? 
Si9 O9 1.592(13) . ? 
Si9 O44 1.661(13) 4_565 ? 
Si10 O26 1.574(14) . ? 
Si10 O10 1.604(14) . ? 
Si10 O9 1.636(13) . ? 
Si10 O41 1.661(13) 4_565 ? 
Si11 O22 1.603(13) . ? 
Si11 O10 1.603(14) . ? 
Si11 O14 1.612(13) . ? 
Si11 O11 1.652(12) . ? 
Si12 O11 1.578(13) . ? 
Si12 O12 1.579(13) . ? 
Si12 O20 1.589(14) . ? 
Si12 O24 1.657(15) . ? 
Si13 O41 1.567(13) . ? 
Si13 O21 1.579(12) 2 ? 
Si13 O27 1.627(12) . ? 
Si13 O42 1.636(13) . ? 
Si14 O27 1.586(13) . ? 
Si14 O39 1.587(14) . ? 
Si14 O32 1.617(13) . ? 
Si14 O28 1.633(13) . ? 
Si15 O28 1.562(12) . ? 
Si15 O29 1.607(12) . ? 
Si15 O19 1.612(12) 4_566 ? 
Si15 O20 1.628(13) 4_566 ? 
Si16 O30 1.593(12) . ? 
Si16 O17 1.599(12) 4_566 ? 
Si16 O29 1.605(12) . ? 
Si16 O16 1.632(12) 4_566 ? 
Si17 O47 1.587(12) . ? 
Si17 O31 1.599(11) . ? 
Si17 O40 1.607(13) . ? 
Si17 O30 1.623(13) . ? 
Si18 O44 1.547(13) . ? 
Si18 O32 1.590(12) . ? 
Si18 O31 1.600(12) . ? 
Si18 O45 1.617(14) . ? 
Si19 O23 1.545(16) . ? 
Si19 O33 1.614(13) . ? 
Si19 O43 1.617(12) . ? 
Si19 O22 1.623(13) 2 ? 
Si20 O34 1.573(13) . ? 
Si20 O39 1.586(14) . ? 
Si20 O33 1.593(14) . ? 
Si20 O38 1.606(14) . ? 
Si21 O18 1.561(13) 4_566 ? 
Si21 O34 1.626(12) . ? 
Si21 O35 1.634(12) . ? 
Si21 O25 1.646(14) . ? 
Si22 O15 1.561(13) 4_566 ? 
Si22 O35 1.587(12) . ? 
Si22 O36 1.592(13) . ? 
Si22 O26 1.646(14) . ? 
Si23 O37 1.576(13) . ? 
Si23 O40 1.583(13) . ? 
Si23 O36 1.595(13) . ? 
Si23 O48 1.615(13) . ? 
Si24 O24 1.545(15) . ? 
Si24 O38 1.616(13) . ? 
Si24 O37 1.618(14) . ? 
Si24 O46 1.640(13) 4_666 ? 
O15 Si22 1.561(13) 4_665 ? 
O16 Si16 1.632(12) 4_665 ? 
O17 Si16 1.598(12) 4_665 ? 
O18 Si21 1.561(13) 4_665 ? 
O19 Si15 1.612(12) 4_665 ? 
O20 Si15 1.628(13) 4_665 ? 
O21 Si13 1.579(12) 2_545 ? 
O22 Si19 1.623(13) 2_545 ? 
O41 Si10 1.661(13) 4_666 ? 
O42 Si4 1.581(12) 4_666 ? 
O43 Si4 1.602(12) 4_666 ? 
O44 Si9 1.661(13) 4_666 ? 
O45 Si3 1.592(13) 4_666 ? 
O46 Si24 1.640(13) 4_565 ? 
O47 Si1 1.633(12) 2_545 ? 
O48 Si7 1.577(13) 2_545 ? 
  
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 
C303 C302 C301 125.4 . . ? 
C302 C303 C304 125.4 . . ? 
C503 C502 C501 125.5 . . ? 
C502 C503 C504 125.4 . . ? 
C103 C101 C102 101(8) 3_675 3_675 ? 
C103 C101 C102 96(6) 3_675 . ? 
C102 C101 C102 52(3) 3_675 . ? 
C103 C101 C104 47(6) 3_675 3_675 ? 
C102 C101 C104 116(4) 3_675 3_675 ? 
C102 C101 C104 75.6(14) . 3_675 ? 
C101 C102 C102 79(3) 3_675 3_675 ? 
C101 C102 C103 20(2) 3_675 . ? 
C102 C102 C103 79(2) 3_675 . ? 
C101 C102 C101 128(3) 3_675 . ? 
C102 C102 C101 50(2) 3_675 . ? 
C103 C102 C101 125.5 . . ? 
C101 C102 C103 129(4) 3_675 3_675 ? 
C102 C102 C103 54.3(16) 3_675 3_675 ? 
C103 C102 C103 133(2) . 3_675 ? 
C101 C102 C103 16.8(18) . 3_675 ? 
C101 C102 C104 148(3) 3_675 3_675 ? 
C102 C102 C104 100(2) 3_675 3_675 ? 
C103 C102 C104 168.4(16) . 3_675 ? 
C101 C102 C104 58.4(17) . 3_675 ? 
C103 C102 C104 47.0(10) 3_675 3_675 ? 
C101 C103 C102 59(6) 3_675 . ? 
C101 C103 C104 119(7) 3_675 . ? 
C102 C103 C104 125.4 . . ? 
C101 C103 C102 67(5) 3_675 3_675 ? 
C102 C103 C102 47(2) . 3_675 ? 
C104 C103 C102 81(2) . 3_675 ? 
C103 C104 C101 13.4(12) . 3_675 ? 
C103 C104 C102 52.3(15) . 3_675 ? 
C101 C104 C102 46.0(12) 3_675 3_675 ? 
C202 C201 C202 80(6) 3_656 . ? 
C202 C201 C201 57(5) 3_656 3_656 ? 
C202 C201 C201 22.6(16) . 3_656 ? 
C202 C201 C203 39(4) 3_656 3_656 ? 
C202 C201 C203 111(2) . 3_656 ? 
C201 C201 C203 90.5(18) 3_656 3_656 ? 
C201 C202 C203 122(5) 3_656 . ? 
C201 C202 C201 100(6) 3_656 . ? 
C203 C202 C201 125.3 . . ? 
C201 C202 C202 74(6) 3_656 3_656 ? 
C203 C202 C202 143.3(13) . 3_656 ? 
C201 C202 C202 26.0(16) . 3_656 ? 
C202 C203 C204 125.5 . . ? 
C202 C203 C201 18.8(17) . 3_656 ? 
C204 C203 C201 137(2) . 3_656 ? 
O16 Si1 O1 109.2(8) . . ? 
O16 Si1 O15 108.6(7) . . ? 
O1 Si1 O15 111.5(8) . . ? 
O16 Si1 O47 109.9(8) . 2 ? 
O1 Si1 O47 107.6(6) . 2 ? 
O15 Si1 O47 110.0(7) . 2 ? 
O6 Si2 O2 108.6(7) . . ? 
O6 Si2 O13 107.5(9) . . ? 
O2 Si2 O13 112.7(8) . . ? 
O6 Si2 O1 111.2(8) . . ? 
O2 Si2 O1 109.0(7) . . ? 
O13 Si2 O1 107.9(9) . . ? 
O46 Si3 O3 108.0(8) . . ? 
O46 Si3 O45 110.6(7) . 4_565 ? 
O3 Si3 O45 110.8(8) . 4_565 ? 
O46 Si3 O2 107.2(8) . . ? 
O3 Si3 O2 109.4(7) . . ? 
O45 Si3 O2 110.7(8) 4_565 . ? 
O42 Si4 O3 113.2(7) 4_565 . ? 
O42 Si4 O43 110.3(7) 4_565 4_565 ? 
O3 Si4 O43 107.7(7) . 4_565 ? 
O42 Si4 O4 108.3(8) 4_565 . ? 
O3 Si4 O4 109.3(7) . . ? 
O43 Si4 O4 107.9(8) 4_565 . ? 
O14 Si5 O4 108.0(7) . . ? 
O14 Si5 O21 111.1(7) . . ? 
O4 Si5 O21 109.1(7) . . ? 
O14 Si5 O5 111.3(7) . . ? 
O4 Si5 O5 110.2(7) . . ? 
O21 Si5 O5 107.1(6) . . ? 
O19 Si6 O5 109.1(7) . . ? 
O19 Si6 O6 111.3(7) . . ? 
O5 Si6 O6 108.8(6) . . ? 
O19 Si6 O18 109.1(7) . . ? 
O5 Si6 O18 107.4(7) . . ? 
O6 Si6 O18 111.1(8) . . ? 
O48 Si7 O7 109.3(7) 2 . ? 
O48 Si7 O17 108.7(7) 2 . ? 
O7 Si7 O17 109.2(8) . . ? 
O48 Si7 O23 111.3(6) 2 . ? 
O7 Si7 O23 110.4(7) . . ? 
O17 Si7 O23 108.0(6) . . ? 
O7 Si8 O13 108.1(9) . . ? 
O7 Si8 O12 111.1(8) . . ? 
O13 Si8 O12 106.8(8) . . ? 
O7 Si8 O8 109.4(8) . . ? 
O13 Si8 O8 111.4(7) . . ? 
O12 Si8 O8 110.1(7) . . ? 
O8 Si9 O25 110.6(6) . . ? 
O8 Si9 O9 108.5(8) . . ? 
O25 Si9 O9 110.3(5) . . ? 
O8 Si9 O44 110.9(7) . 4_565 ? 
O25 Si9 O44 108.5(6) . 4_565 ? 
O9 Si9 O44 108.0(8) . 4_565 ? 
O26 Si10 O10 109.8(6) . . ? 
O26 Si10 O9 110.4(5) . . ? 
O10 Si10 O9 107.9(8) . . ? 
O26 Si10 O41 107.5(6) . 4_565 ? 
O10 Si10 O41 112.3(8) . 4_565 ? 
O9 Si10 O41 108.9(8) . 4_565 ? 
O22 Si11 O10 110.8(8) . . ? 
O22 Si11 O14 110.8(7) . . ? 
O10 Si11 O14 108.7(7) . . ? 
O22 Si11 O11 105.5(6) . . ? 
O10 Si11 O11 112.1(7) . . ? 
O14 Si11 O11 109.0(7) . . ? 
O11 Si12 O12 111.0(7) . . ? 
O11 Si12 O20 106.1(7) . . ? 
O12 Si12 O20 109.8(7) . . ? 
O11 Si12 O24 109.8(6) . . ? 
O12 Si12 O24 111.6(6) . . ? 
O20 Si12 O24 108.4(6) . . ? 
O41 Si13 O21 107.2(7) . 2 ? 
O41 Si13 O27 108.5(8) . . ? 
O21 Si13 O27 109.5(6) 2 . ? 
O41 Si13 O42 109.5(7) . . ? 
O21 Si13 O42 109.3(7) 2 . ? 
O27 Si13 O42 112.6(7) . . ? 
O27 Si14 O39 111.2(8) . . ? 
O27 Si14 O32 108.2(8) . . ? 
O39 Si14 O32 110.6(9) . . ? 
O27 Si14 O28 108.2(7) . . ? 
O39 Si14 O28 108.8(8) . . ? 
O32 Si14 O28 109.8(7) . . ? 
O28 Si15 O29 112.1(7) . . ? 
O28 Si15 O19 107.9(8) . 4_566 ? 
O29 Si15 O19 106.4(7) . 4_566 ? 
O28 Si15 O20 109.9(8) . 4_566 ? 
O29 Si15 O20 111.6(7) . 4_566 ? 
O19 Si15 O20 108.8(7) 4_566 4_566 ? 
O30 Si16 O17 108.3(8) . 4_566 ? 
O30 Si16 O29 111.3(7) . . ? 
O17 Si16 O29 111.7(7) 4_566 . ? 
O30 Si16 O16 111.4(8) . 4_566 ? 
O17 Si16 O16 109.9(7) 4_566 4_566 ? 
O29 Si16 O16 104.2(8) . 4_566 ? 
O47 Si17 O31 107.9(6) . . ? 
O47 Si17 O40 110.4(7) . . ? 
O31 Si17 O40 109.4(7) . . ? 
O47 Si17 O30 111.4(7) . . ? 
O31 Si17 O30 108.9(6) . . ? 
O40 Si17 O30 108.7(7) . . ? 
O44 Si18 O32 108.4(8) . . ? 
O44 Si18 O31 108.6(7) . . ? 
O32 Si18 O31 110.1(6) . . ? 
O44 Si18 O45 109.5(8) . . ? 
O32 Si18 O45 109.9(8) . . ? 
O31 Si18 O45 110.2(8) . . ? 
O23 Si19 O33 109.5(6) . . ? 
O23 Si19 O43 107.6(6) . . ? 
O33 Si19 O43 111.5(7) . . ? 
O23 Si19 O22 110.0(6) . 2 ? 
O33 Si19 O22 106.2(7) . 2 ? 
O43 Si19 O22 112.0(7) . 2 ? 
O34 Si20 O39 108.6(8) . . ? 
O34 Si20 O33 106.3(7) . . ? 
O39 Si20 O33 111.5(8) . . ? 
O34 Si20 O38 109.0(7) . . ? 
O39 Si20 O38 112.0(8) . . ? 
O33 Si20 O38 109.3(8) . . ? 
O18 Si21 O34 109.2(7) 4_566 . ? 
O18 Si21 O35 110.5(7) 4_566 . ? 
O34 Si21 O35 109.2(7) . . ? 
O18 Si21 O25 107.7(6) 4_566 . ? 
O34 Si21 O25 109.1(6) . . ? 
O35 Si21 O25 111.1(5) . . ? 
O15 Si22 O35 109.4(7) 4_566 . ? 
O15 Si22 O36 109.8(8) 4_566 . ? 
O35 Si22 O36 108.8(8) . . ? 
O15 Si22 O26 109.2(6) 4_566 . ? 
O35 Si22 O26 110.7(5) . . ? 
O36 Si22 O26 108.7(6) . . ? 
O37 Si23 O40 110.6(7) . . ? 
O37 Si23 O36 107.8(7) . . ? 
O40 Si23 O36 109.0(8) . . ? 
O37 Si23 O48 111.1(7) . . ? 
O40 Si23 O48 109.7(7) . . ? 
O36 Si23 O48 108.5(7) . . ? 
O24 Si24 O38 107.9(6) . . ? 
O24 Si24 O37 109.9(6) . . ? 
O38 Si24 O37 106.1(7) . . ? 
O24 Si24 O46 107.1(6) . 4_666 ? 
O38 Si24 O46 111.7(7) . 4_666 ? 
O37 Si24 O46 114.0(7) . 4_666 ? 
Si1 O1 Si2 155.4(10) . . ? 
Si2 O2 Si3 151.5(9) . . ? 
Si4 O3 Si3 178.1(11) . . ? 
Si5 O4 Si4 155.9(10) . . ? 
Si6 O5 Si5 146.1(8) . . ? 
Si2 O6 Si6 161.1(10) . . ? 
Si8 O7 Si7 160.7(10) . . ? 
Si9 O8 Si8 156.9(10) . . ? 
Si9 O9 Si10 152.6(8) . . ? 
Si11 O10 Si10 162.1(10) . . ? 
Si12 O11 Si11 147.4(8) . . ? 
Si12 O12 Si8 167.4(10) . . ? 
Si8 O13 Si2 177.3(12) . . ? 
Si5 O14 Si11 165.8(10) . . ? 
Si22 O15 Si1 148.0(9) 4_665 . ? 
Si1 O16 Si16 167.7(11) . 4_665 ? 
Si16 O17 Si7 147.2(9) 4_665 . ? 
Si21 O18 Si6 143.7(8) 4_665 . ? 
Si6 O19 Si15 159.4(9) . 4_665 ? 
Si12 O20 Si15 148.5(10) . 4_665 ? 
Si13 O21 Si5 148.5(8) 2_545 . ? 
Si11 O22 Si19 147.4(8) . 2_545 ? 
Si19 O23 Si7 155.3(3) . . ? 
Si24 O24 Si12 150.0(3) . . ? 
Si9 O25 Si21 153.1(3) . . ? 
Si10 O26 Si22 145.9(3) . . ? 
Si14 O27 Si13 153.2(10) . . ? 
Si15 O28 Si14 153.2(10) . . ? 
Si16 O29 Si15 167.2(10) . . ? 
Si16 O30 Si17 155.2(9) . . ? 
Si17 O31 Si18 147.8(8) . . ? 
Si18 O32 Si14 159.8(10) . . ? 
Si20 O33 Si19 155.8(10) . . ? 
Si20 O34 Si21 155.1(9) . . ? 
Si22 O35 Si21 151.3(8) . . ? 
Si22 O36 Si23 162.9(11) . . ? 
Si23 O37 Si24 155.2(10) . . ? 
Si20 O38 Si24 162.5(10) . . ? 
Si20 O39 Si14 177.8(11) . . ? 
Si23 O40 Si17 165.7(9) . . ? 
Si13 O41 Si10 147.2(9) . 4_666 ? 
Si4 O42 Si13 161.7(10) 4_666 . ? 
Si4 O43 Si19 147.7(9) 4_666 . ? 
Si18 O44 Si9 146.7(9) . 4_666 ? 
Si3 O45 Si18 163.2(11) 4_666 . ? 
Si3 O46 Si24 147.4(9) . 4_565 ? 
Si17 O47 Si1 147.1(8) . 2_545 ? 
Si7 O48 Si23 153.2(9) 2_545 . ? 
  
_diffrn_measured_fraction_theta_max    0.936 
_diffrn_reflns_theta_full              28.75 
_diffrn_measured_fraction_theta_full   0.936 
_refine_diff_density_max    0.862 
_refine_diff_density_min   -0.573 
_refine_diff_density_rms    0.127 




  
data_f_ip_twin_7d_mo 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C10 H0 O48 Si24' 
_chemical_formula_weight          1562 
  
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' 
 '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' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    13.435(19) 
_cell_length_b                    20.16(3) 
_cell_length_c                    19.90(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      5390(13) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.21 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.866 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3048 
_exptl_absorpt_coefficient_mu     0.673 
_exptl_absorpt_correction_type    Analytical 
_exptl_absorpt_correction_T_min   0.8722 
_exptl_absorpt_correction_T_max   0.9563 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       296(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   'Bruker P4' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             62763 
_diffrn_reflns_av_R_equivalents   0.1070 
_diffrn_reflns_av_sigmaI/netI     0.1285 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        27 
_diffrn_reflns_limit_l_min        -26 
_diffrn_reflns_limit_l_max        26 
_diffrn_reflns_theta_min          1.01 
_diffrn_reflns_theta_max          28.63 
_reflns_number_total              13020 
_reflns_number_gt                 5815 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker XSCANS' 
_computing_cell_refinement        'Bruker XSCANS' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_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)+(0.0490P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none 
_refine_ls_hydrogen_treatment     none 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          13020 
_refine_ls_number_parameters      692 
_refine_ls_number_restraints      16 
_refine_ls_R_factor_all           0.1269 
_refine_ls_R_factor_gt            0.0520 
_refine_ls_wR_factor_ref          0.1336 
_refine_ls_wR_factor_gt           0.1144 
_refine_ls_goodness_of_fit_ref    0.821 
_refine_ls_restrained_S_all       0.854 
_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 
C101 C 0.557(5) 0.012(3) 0.1573(19) 0.70(5) Uiso 1 1 d D A 1 
C102 C 0.596(2) 0.0043(15) 0.230(2) 0.45(2) Uiso 1 1 d D A 1 
C103 C 0.492(2) -0.0029(13) 0.2672(19) 0.376(18) Uiso 1 1 d D A 1 
C104 C 0.522(3) 0.005(2) 0.3431(18) 0.46(3) Uiso 1 1 d D A 1 
C105 C 0.615(3) 0.0853(18) 0.250(3) 0.65(3) Uiso 1 1 d D A 1 
C201 C 0.0381(14) 0.2045(8) 0.7678(11) 0.228(9) Uiso 1 1 d D B 2 
C202 C 0.1371(16) 0.2009(9) 0.7289(11) 0.229(10) Uiso 1 1 d D B 2 
C203 C 0.1925(12) 0.1408(8) 0.7535(14) 0.216(8) Uiso 1 1 d D B 2 
C204 C 0.1392(12) 0.0709(8) 0.7491(17) 0.213(7) Uiso 1 1 d D B 2 
C205 C 0.1940(12) 0.2720(8) 0.7480(14) 0.215(8) Uiso 1 1 d D B 2 
Si1 Si 0.32720(17) 0.42119(10) -0.05642(14) 0.0151(5) Uani 1 1 d . . . 
Si2 Si 0.17683(18) 0.30980(12) -0.02988(10) 0.0177(5) Uani 1 1 d . . . 
Si3 Si -0.04218(17) 0.27998(11) -0.06249(13) 0.0170(5) Uani 1 1 d . . . 
Si4 Si -0.03227(16) 0.12334(11) -0.06303(12) 0.0148(5) Uani 1 1 d . . . 
Si5 Si 0.17959(19) 0.07461(11) -0.02805(11) 0.0153(5) Uani 1 1 d . . . 
Si6 Si 0.32308(17) 0.19006(11) -0.05625(12) 0.0171(5) Uani 1 1 d . . . 
Si7 Si 0.32399(19) 0.42415(11) 0.17126(12) 0.0155(5) Uani 1 1 d . . . 
Si8 Si 0.18280(17) 0.30907(12) 0.12764(11) 0.0170(5) Uani 1 1 d . . . 
Si9 Si -0.02923(17) 0.27382(12) 0.17601(11) 0.0159(5) Uani 1 1 d . . . 
Si10 Si -0.02840(18) 0.11998(12) 0.17593(11) 0.0172(6) Uani 1 1 d . . . 
Si11 Si 0.18116(19) 0.07127(11) 0.12976(12) 0.0161(5) Uani 1 1 d . . . 
Si12 Si 0.32071(18) 0.18816(12) 0.16807(11) 0.0163(5) Uani 1 1 d . . . 
Si13 Si 0.33855(16) 0.42626(10) 0.55860(14) 0.0149(5) Uani 1 1 d . . . 
Si14 Si 0.19428(17) 0.30974(13) 0.52905(10) 0.0165(5) Uani 1 1 d . . . 
Si15 Si -0.02626(16) 0.27867(11) 0.56182(12) 0.0153(5) Uani 1 1 d . . . 
Si16 Si -0.02933(17) 0.12166(11) 0.56373(13) 0.0160(5) Uani 1 1 d . . . 
Si17 Si 0.18440(18) 0.07115(11) 0.52848(11) 0.0142(5) Uani 1 1 d . . . 
Si18 Si 0.32698(17) 0.18602(11) 0.56251(12) 0.0165(5) Uani 1 1 d . . . 
Si19 Si 0.31998(19) 0.42397(11) 0.32774(12) 0.0166(5) Uani 1 1 d . . . 
Si20 Si 0.17970(18) 0.31018(12) 0.37076(12) 0.0167(5) Uani 1 1 d . . . 
Si21 Si -0.03618(18) 0.27417(12) 0.33147(11) 0.0166(5) Uani 1 1 d . . . 
Si22 Si -0.03300(18) 0.11916(12) 0.32985(11) 0.0169(5) Uani 1 1 d . . . 
Si23 Si 0.18017(19) 0.07108(10) 0.37047(12) 0.0156(5) Uani 1 1 d . . . 
Si24 Si 0.30881(18) 0.18957(12) 0.32261(10) 0.0167(5) Uani 1 1 d . . . 
O1 O 0.2318(4) 0.3745(3) -0.0564(4) 0.0381(16) Uani 1 1 d . . . 
O2 O 0.0692(4) 0.3067(3) -0.0639(3) 0.0304(14) Uani 1 1 d . . . 
O3 O -0.0434(5) 0.2017(3) -0.0546(3) 0.0423(15) Uani 1 1 d . . . 
O4 O 0.0828(4) 0.1039(3) -0.0645(3) 0.0288(15) Uani 1 1 d . . . 
O5 O 0.2745(4) 0.1179(3) -0.0488(3) 0.0252(14) Uani 1 1 d . . . 
O6 O 0.2379(4) 0.2448(3) -0.0493(4) 0.0392(17) Uani 1 1 d . . . 
O7 O 0.2344(5) 0.3736(3) 0.1542(3) 0.0389(19) Uani 1 1 d . . . 
O8 O 0.0781(4) 0.3036(3) 0.1650(3) 0.0329(15) Uani 1 1 d . . . 
O9 O -0.0292(5) 0.1968(3) 0.1558(2) 0.0346(17) Uani 1 1 d . . . 
O10 O 0.0819(5) 0.0916(3) 0.1679(3) 0.0350(16) Uani 1 1 d . . . 
O11 O 0.2705(5) 0.1196(3) 0.1509(3) 0.0288(16) Uani 1 1 d . . . 
O12 O 0.2476(5) 0.2459(3) 0.1435(3) 0.0418(19) Uani 1 1 d . . . 
O13 O 0.1654(5) 0.3140(3) 0.0497(3) 0.0491(17) Uani 1 1 d . . . 
O14 O 0.1628(4) 0.0778(3) 0.0505(3) 0.0317(14) Uani 1 1 d . . . 
O15 O 0.3809(4) 0.4138(3) -0.1266(3) 0.0323(16) Uani 1 1 d . . . 
O16 O 0.4024(5) 0.4017(3) 0.0034(3) 0.0440(19) Uani 1 1 d . . . 
O17 O 0.4219(5) 0.4015(3) 0.1324(3) 0.0301(16) Uani 1 1 d . . . 
O18 O 0.3718(4) 0.1954(3) -0.1293(3) 0.0296(14) Uani 1 1 d . . . 
O19 O 0.4093(5) 0.1999(3) -0.0010(3) 0.0370(16) Uani 1 1 d . . . 
O20 O 0.4236(4) 0.1951(3) 0.1291(3) 0.0271(14) Uani 1 1 d . . . 
O21 O 0.2019(4) 0.0001(2) -0.0526(3) 0.0249(13) Uani 1 1 d . . . 
O22 O 0.2115(4) -0.0027(3) 0.1491(3) 0.0252(15) Uani 1 1 d . . . 
O23 O 0.3467(3) 0.4228(2) 0.2500(4) 0.0310(11) Uani 1 1 d . . . 
O24 O 0.3437(3) 0.1935(2) 0.2469(3) 0.0288(10) Uani 1 1 d . . . 
O25 O -0.0568(3) 0.28349(18) 0.2528(3) 0.0254(10) Uani 1 1 d . . . 
O26 O -0.0622(3) 0.11036(18) 0.2517(3) 0.0222(10) Uani 1 1 d . . . 
O27 O 0.2470(4) 0.3754(3) 0.5543(4) 0.0345(16) Uani 1 1 d . . . 
O28 O 0.0817(4) 0.3097(3) 0.5561(3) 0.0288(13) Uani 1 1 d . . . 
O29 O -0.0190(5) 0.2002(3) 0.5633(3) 0.0475(18) Uani 1 1 d . . . 
O30 O 0.0767(4) 0.0885(3) 0.5576(3) 0.0343(15) Uani 1 1 d . . . 
O31 O 0.2664(4) 0.1179(3) 0.5624(3) 0.0271(14) Uani 1 1 d . . . 
O32 O 0.2520(4) 0.2473(3) 0.5587(3) 0.0332(15) Uani 1 1 d . . . 
O33 O 0.2291(5) 0.3763(3) 0.3419(3) 0.0339(18) Uani 1 1 d . . . 
O34 O 0.0644(4) 0.3116(3) 0.3546(2) 0.0243(13) Uani 1 1 d . . . 
O35 O -0.0255(5) 0.1964(3) 0.3482(2) 0.0289(15) Uani 1 1 d . . . 
O36 O 0.0701(5) 0.0849(3) 0.3448(3) 0.0409(18) Uani 1 1 d . . . 
O37 O 0.2585(5) 0.1185(3) 0.3340(3) 0.0377(18) Uani 1 1 d . . . 
O38 O 0.2292(5) 0.2463(3) 0.3362(3) 0.0413(18) Uani 1 1 d . . . 
O39 O 0.1977(4) 0.3059(3) 0.4495(3) 0.0526(17) Uani 1 1 d . . . 
O40 O 0.1838(5) 0.0820(3) 0.4493(3) 0.0386(15) Uani 1 1 d . . . 
O41 O 0.3955(5) 0.4198(3) 0.6286(3) 0.0332(16) Uani 1 1 d . . . 
O42 O 0.4131(5) 0.4115(3) 0.4993(3) 0.0317(15) Uani 1 1 d . . . 
O43 O 0.4173(4) 0.3999(3) 0.3679(3) 0.0304(16) Uani 1 1 d . . . 
O44 O 0.3896(4) 0.1891(3) 0.6301(3) 0.0244(13) Uani 1 1 d . . . 
O45 O 0.4007(4) 0.1870(3) 0.4996(3) 0.0307(15) Uani 1 1 d . . . 
O46 O -0.0946(4) 0.3015(3) -0.1307(3) 0.0408(17) Uani 1 1 d . . . 
O47 O 0.2093(4) -0.0041(2) 0.5463(3) 0.0253(14) Uani 1 1 d . . . 
O48 O 0.2092(5) -0.0037(3) 0.3523(3) 0.0318(16) Uani 1 1 d . . . 
  
  
_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 
C101 C102 1.55(2) . ? 
C102 C103 1.58(2) . ? 
C102 C105 1.698(18) . ? 
C103 C104 1.568(19) . ? 
C201 C202 1.541(17) . ? 
C202 C203 1.503(16) . ? 
C202 C205 1.668(15) . ? 
C203 C204 1.583(14) . ? 
Si1 O15 1.578(7) . ? 
Si1 O1 1.589(6) . ? 
Si1 O47 1.597(6) 2 ? 
Si1 O16 1.610(7) . ? 
Si2 O1 1.590(6) . ? 
Si2 O6 1.594(6) . ? 
Si2 O13 1.594(6) . ? 
Si2 O2 1.598(6) . ? 
Si3 O3 1.586(6) . ? 
Si3 O2 1.590(6) . ? 
Si3 O46 1.590(6) . ? 
Si3 O45 1.599(6) 4_565 ? 
Si4 O4 1.595(6) . ? 
Si4 O3 1.595(6) . ? 
Si4 O42 1.603(6) 4_565 ? 
Si4 O43 1.603(6) 4_565 ? 
Si5 O14 1.581(7) . ? 
Si5 O5 1.599(6) . ? 
Si5 O4 1.603(6) . ? 
Si5 O21 1.607(6) . ? 
Si6 O6 1.595(6) . ? 
Si6 O18 1.598(6) . ? 
Si6 O5 1.602(6) . ? 
Si6 O19 1.609(6) . ? 
Si7 O48 1.591(7) 2 ? 
Si7 O17 1.593(7) . ? 
Si7 O23 1.598(8) . ? 
Si7 O7 1.613(6) . ? 
Si8 O7 1.566(6) . ? 
Si8 O13 1.571(6) . ? 
Si8 O12 1.576(6) . ? 
Si8 O8 1.595(6) . ? 
Si9 O8 1.578(6) . ? 
Si9 O25 1.584(7) . ? 
Si9 O9 1.604(6) . ? 
Si9 O44 1.607(6) 4_565 ? 
Si10 O26 1.587(7) . ? 
Si10 O10 1.597(7) . ? 
Si10 O9 1.600(6) . ? 
Si10 O41 1.605(6) 4_565 ? 
Si11 O10 1.587(7) . ? 
Si11 O22 1.592(6) . ? 
Si11 O11 1.602(6) . ? 
Si11 O14 1.602(7) . ? 
Si12 O11 1.576(6) . ? 
Si12 O20 1.591(6) . ? 
Si12 O12 1.599(6) . ? 
Si12 O24 1.603(7) . ? 
Si13 O42 1.576(7) . ? 
Si13 O21 1.590(5) 2 ? 
Si13 O41 1.595(7) . ? 
Si13 O27 1.604(6) . ? 
Si14 O27 1.583(6) . ? 
Si14 O39 1.585(6) . ? 
Si14 O32 1.591(6) . ? 
Si14 O28 1.606(6) . ? 
Si15 O19 1.582(6) 4_566 ? 
Si15 O28 1.583(6) . ? 
Si15 O29 1.584(6) . ? 
Si15 O20 1.589(6) 4_566 ? 
Si16 O30 1.577(6) . ? 
Si16 O16 1.582(6) 4_566 ? 
Si16 O17 1.586(6) 4_566 ? 
Si16 O29 1.590(6) . ? 
Si17 O40 1.591(7) . ? 
Si17 O47 1.593(6) . ? 
Si17 O30 1.598(6) . ? 
Si17 O31 1.599(6) . ? 
Si18 O44 1.587(6) . ? 
Si18 O31 1.596(6) . ? 
Si18 O32 1.596(6) . ? 
Si18 O45 1.597(6) . ? 
Si19 O33 1.580(6) . ? 
Si19 O23 1.587(8) . ? 
Si19 O22 1.606(6) 2 ? 
Si19 O43 1.606(6) . ? 
Si20 O34 1.583(6) . ? 
Si20 O39 1.588(6) . ? 
Si20 O33 1.596(6) . ? 
Si20 O38 1.603(6) . ? 
Si21 O18 1.585(6) 4_566 ? 
Si21 O25 1.601(7) . ? 
Si21 O35 1.610(6) . ? 
Si21 O34 1.614(6) . ? 
Si22 O36 1.576(7) . ? 
Si22 O15 1.591(6) 4_566 ? 
Si22 O35 1.602(6) . ? 
Si22 O26 1.614(7) . ? 
Si23 O40 1.585(7) . ? 
Si23 O36 1.589(7) . ? 
Si23 O37 1.597(6) . ? 
Si23 O48 1.599(7) . ? 
Si24 O24 1.579(6) . ? 
Si24 O38 1.590(6) . ? 
Si24 O37 1.600(7) . ? 
Si24 O46 1.605(6) 4_666 ? 
O15 Si22 1.591(6) 4_665 ? 
O16 Si16 1.582(6) 4_665 ? 
O17 Si16 1.586(6) 4_665 ? 
O18 Si21 1.585(6) 4_665 ? 
O19 Si15 1.582(6) 4_665 ? 
O20 Si15 1.589(6) 4_665 ? 
O21 Si13 1.590(5) 2_545 ? 
O22 Si19 1.606(6) 2_545 ? 
O41 Si10 1.605(6) 4_666 ? 
O42 Si4 1.603(6) 4_666 ? 
O43 Si4 1.604(6) 4_666 ? 
O44 Si9 1.607(6) 4_666 ? 
O45 Si3 1.599(6) 4_666 ? 
O46 Si24 1.605(6) 4_565 ? 
O47 Si1 1.597(6) 2_545 ? 
O48 Si7 1.592(7) 2_545 ? 
  
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 
C101 C102 C103 98(2) . . ? 
C101 C102 C105 100(2) . . ? 
C103 C102 C105 96(2) . . ? 
C104 C103 C102 103(3) . . ? 
C203 C202 C201 107.6(17) . . ? 
C203 C202 C205 113.1(16) . . ? 
C201 C202 C205 103.9(15) . . ? 
C202 C203 C204 118.4(17) . . ? 
O15 Si1 O1 108.2(4) . . ? 
O15 Si1 O47 109.9(3) . 2 ? 
O1 Si1 O47 108.1(3) . 2 ? 
O15 Si1 O16 110.1(4) . . ? 
O1 Si1 O16 111.2(4) . . ? 
O47 Si1 O16 109.3(4) 2 . ? 
O1 Si2 O6 110.8(4) . . ? 
O1 Si2 O13 109.3(4) . . ? 
O6 Si2 O13 109.5(4) . . ? 
O1 Si2 O2 108.2(3) . . ? 
O6 Si2 O2 109.4(3) . . ? 
O13 Si2 O2 109.6(3) . . ? 
O3 Si3 O2 110.4(3) . . ? 
O3 Si3 O46 110.6(4) . . ? 
O2 Si3 O46 108.1(4) . . ? 
O3 Si3 O45 109.5(4) . 4_565 ? 
O2 Si3 O45 108.9(3) . 4_565 ? 
O46 Si3 O45 109.4(4) . 4_565 ? 
O4 Si4 O3 109.6(3) . . ? 
O4 Si4 O42 110.5(4) . 4_565 ? 
O3 Si4 O42 108.1(4) . 4_565 ? 
O4 Si4 O43 108.8(4) . 4_565 ? 
O3 Si4 O43 109.9(4) . 4_565 ? 
O42 Si4 O43 109.9(3) 4_565 4_565 ? 
O14 Si5 O5 110.3(3) . . ? 
O14 Si5 O4 108.5(3) . . ? 
O5 Si5 O4 109.2(3) . . ? 
O14 Si5 O21 111.4(3) . . ? 
O5 Si5 O21 106.4(3) . . ? 
O4 Si5 O21 110.9(3) . . ? 
O6 Si6 O18 109.0(4) . . ? 
O6 Si6 O5 109.2(3) . . ? 
O18 Si6 O5 108.2(3) . . ? 
O6 Si6 O19 111.8(4) . . ? 
O18 Si6 O19 108.5(4) . . ? 
O5 Si6 O19 110.0(3) . . ? 
O48 Si7 O17 110.5(4) 2 . ? 
O48 Si7 O23 111.0(3) 2 . ? 
O17 Si7 O23 108.3(3) . . ? 
O48 Si7 O7 107.9(4) 2 . ? 
O17 Si7 O7 109.5(4) . . ? 
O23 Si7 O7 109.8(3) . . ? 
O7 Si8 O13 110.3(4) . . ? 
O7 Si8 O12 111.1(4) . . ? 
O13 Si8 O12 109.4(3) . . ? 
O7 Si8 O8 106.9(4) . . ? 
O13 Si8 O8 109.5(3) . . ? 
O12 Si8 O8 109.8(4) . . ? 
O8 Si9 O25 107.5(3) . . ? 
O8 Si9 O9 109.5(3) . . ? 
O25 Si9 O9 111.2(3) . . ? 
O8 Si9 O44 111.4(3) . 4_565 ? 
O25 Si9 O44 109.4(3) . 4_565 ? 
O9 Si9 O44 107.9(3) . 4_565 ? 
O26 Si10 O10 108.5(3) . . ? 
O26 Si10 O9 110.7(3) . . ? 
O10 Si10 O9 109.2(4) . . ? 
O26 Si10 O41 108.3(3) . 4_565 ? 
O10 Si10 O41 110.7(4) . 4_565 ? 
O9 Si10 O41 109.4(3) . 4_565 ? 
O10 Si11 O22 109.9(4) . . ? 
O10 Si11 O11 110.3(4) . . ? 
O22 Si11 O11 108.3(3) . . ? 
O10 Si11 O14 108.6(3) . . ? 
O22 Si11 O14 110.8(3) . . ? 
O11 Si11 O14 108.9(3) . . ? 
O11 Si12 O20 110.1(3) . . ? 
O11 Si12 O12 108.0(4) . . ? 
O20 Si12 O12 108.7(3) . . ? 
O11 Si12 O24 110.7(3) . . ? 
O20 Si12 O24 107.7(3) . . ? 
O12 Si12 O24 111.6(3) . . ? 
O42 Si13 O21 109.7(3) . 2 ? 
O42 Si13 O41 109.5(4) . . ? 
O21 Si13 O41 107.8(3) 2 . ? 
O42 Si13 O27 109.1(4) . . ? 
O21 Si13 O27 109.4(3) 2 . ? 
O41 Si13 O27 111.3(4) . . ? 
O27 Si14 O39 110.2(4) . . ? 
O27 Si14 O32 109.0(3) . . ? 
O39 Si14 O32 108.5(4) . . ? 
O27 Si14 O28 108.4(3) . . ? 
O39 Si14 O28 111.2(3) . . ? 
O32 Si14 O28 109.5(3) . . ? 
O19 Si15 O28 109.7(4) 4_566 . ? 
O19 Si15 O29 108.7(4) 4_566 . ? 
O28 Si15 O29 109.8(3) . . ? 
O19 Si15 O20 110.1(3) 4_566 4_566 ? 
O28 Si15 O20 108.5(3) . 4_566 ? 
O29 Si15 O20 110.0(4) . 4_566 ? 
O30 Si16 O16 109.8(4) . 4_566 ? 
O30 Si16 O17 108.3(4) . 4_566 ? 
O16 Si16 O17 109.1(4) 4_566 4_566 ? 
O30 Si16 O29 110.1(3) . . ? 
O16 Si16 O29 110.1(4) 4_566 . ? 
O17 Si16 O29 109.5(3) 4_566 . ? 
O40 Si17 O47 110.7(3) . . ? 
O40 Si17 O30 109.0(4) . . ? 
O47 Si17 O30 108.5(3) . . ? 
O40 Si17 O31 109.9(3) . . ? 
O47 Si17 O31 108.8(3) . . ? 
O30 Si17 O31 109.9(4) . . ? 
O44 Si18 O31 107.8(3) . . ? 
O44 Si18 O32 110.2(3) . . ? 
O31 Si18 O32 110.1(3) . . ? 
O44 Si18 O45 109.6(3) . . ? 
O31 Si18 O45 109.0(3) . . ? 
O32 Si18 O45 110.2(3) . . ? 
O33 Si19 O23 109.8(3) . . ? 
O33 Si19 O22 107.8(4) . 2 ? 
O23 Si19 O22 110.7(3) . 2 ? 
O33 Si19 O43 110.9(4) . . ? 
O23 Si19 O43 107.2(3) . . ? 
O22 Si19 O43 110.4(3) 2 . ? 
O34 Si20 O39 110.5(3) . . ? 
O34 Si20 O33 108.6(3) . . ? 
O39 Si20 O33 109.8(4) . . ? 
O34 Si20 O38 109.5(3) . . ? 
O39 Si20 O38 108.4(4) . . ? 
O33 Si20 O38 110.1(4) . . ? 
O18 Si21 O25 107.5(3) 4_566 . ? 
O18 Si21 O35 110.1(4) 4_566 . ? 
O25 Si21 O35 109.4(3) . . ? 
O18 Si21 O34 109.4(3) 4_566 . ? 
O25 Si21 O34 111.6(3) . . ? 
O35 Si21 O34 108.8(3) . . ? 
O36 Si22 O15 110.6(4) . 4_566 ? 
O36 Si22 O35 109.2(4) . . ? 
O15 Si22 O35 109.1(3) 4_566 . ? 
O36 Si22 O26 110.3(3) . . ? 
O15 Si22 O26 107.6(3) 4_566 . ? 
O35 Si22 O26 110.0(3) . . ? 
O40 Si23 O36 108.8(4) . . ? 
O40 Si23 O37 110.3(3) . . ? 
O36 Si23 O37 111.2(4) . . ? 
O40 Si23 O48 110.4(3) . . ? 
O36 Si23 O48 108.6(4) . . ? 
O37 Si23 O48 107.5(4) . . ? 
O24 Si24 O38 109.0(3) . . ? 
O24 Si24 O37 107.8(3) . . ? 
O38 Si24 O37 109.6(4) . . ? 
O24 Si24 O46 107.8(3) . 4_666 ? 
O38 Si24 O46 111.4(4) . 4_666 ? 
O37 Si24 O46 111.1(4) . 4_666 ? 
Si1 O1 Si2 149.4(5) . . ? 
Si3 O2 Si2 149.1(4) . . ? 
Si3 O3 Si4 166.9(5) . . ? 
Si4 O4 Si5 150.3(4) . . ? 
Si5 O5 Si6 147.6(4) . . ? 
Si2 O6 Si6 163.5(5) . . ? 
Si8 O7 Si7 157.8(5) . . ? 
Si9 O8 Si8 153.8(4) . . ? 
Si10 O9 Si9 151.0(3) . . ? 
Si11 O10 Si10 156.9(4) . . ? 
Si12 O11 Si11 155.7(5) . . ? 
Si8 O12 Si12 171.6(5) . . ? 
Si8 O13 Si2 164.4(5) . . ? 
Si5 O14 Si11 161.5(4) . . ? 
Si1 O15 Si22 148.6(4) . 4_665 ? 
Si16 O16 Si1 175.8(5) 4_665 . ? 
Si16 O17 Si7 147.5(4) 4_665 . ? 
Si21 O18 Si6 142.5(4) 4_665 . ? 
Si15 O19 Si6 165.4(5) 4_665 . ? 
Si15 O20 Si12 143.9(4) 4_665 . ? 
Si13 O21 Si5 146.5(4) 2_545 . ? 
Si11 O22 Si19 149.8(4) . 2_545 ? 
Si19 O23 Si7 155.8(3) . . ? 
Si24 O24 Si12 150.8(3) . . ? 
Si9 O25 Si21 152.7(3) . . ? 
Si10 O26 Si22 146.4(3) . . ? 
Si14 O27 Si13 153.4(5) . . ? 
Si15 O28 Si14 152.6(4) . . ? 
Si15 O29 Si16 171.5(5) . . ? 
Si16 O30 Si17 159.7(5) . . ? 
Si18 O31 Si17 149.2(4) . . ? 
Si14 O32 Si18 159.6(5) . . ? 
Si19 O33 Si20 153.4(5) . . ? 
Si20 O34 Si21 150.3(4) . . ? 
Si22 O35 Si21 153.4(4) . . ? 
Si22 O36 Si23 162.8(5) . . ? 
Si23 O37 Si24 151.5(5) . . ? 
Si24 O38 Si20 158.4(5) . . ? 
Si14 O39 Si20 168.0(4) . . ? 
Si23 O40 Si17 164.0(4) . . ? 
Si13 O41 Si10 149.2(4) . 4_666 ? 
Si13 O42 Si4 162.3(5) . 4_666 ? 
Si4 O43 Si19 149.2(4) 4_666 . ? 
Si18 O44 Si9 149.3(4) . 4_666 ? 
Si18 O45 Si3 155.3(5) . 4_666 ? 
Si3 O46 Si24 152.0(4) . 4_565 ? 
Si17 O47 Si1 149.5(4) . 2_545 ? 
Si7 O48 Si23 149.4(5) 2_545 . ? 
  
_diffrn_measured_fraction_theta_max    0.940 
_diffrn_reflns_theta_full              28.63 
_diffrn_measured_fraction_theta_full   0.940 
_refine_diff_density_max    0.904 
_refine_diff_density_min   -0.566 
_refine_diff_density_rms    0.142 




  
data_f_butane_twin_70h 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C8  O48 Si24' 
_chemical_formula_weight          1538 
  
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' 
 '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' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    13.418(5) 
_cell_length_b                    20.131(7) 
_cell_length_c                    19.924(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.060(13) 
_cell_angle_gamma                 90.00 
_cell_volume                      5382(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.23 
_exptl_crystal_size_mid           0.11 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.852 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3016 
_exptl_absorpt_coefficient_mu     0.673 
_exptl_absorpt_correction_type    Analytical
_exptl_absorpt_correction_T_min   0.8623 
_exptl_absorpt_correction_T_max   0.9538 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       296(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   'Bruker P4' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             63839 
_diffrn_reflns_av_R_equivalents   0.1438 
_diffrn_reflns_av_sigmaI/netI     0.1230 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        -24 
_diffrn_reflns_limit_k_max        23 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        25 
_diffrn_reflns_theta_min          1.52 
_diffrn_reflns_theta_max          29.58 
_reflns_number_total              12710 
_reflns_number_gt                 6752 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker XSCANS' 
_computing_cell_refinement        'Bruker XSCANS' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_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)+(0.0549P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none
_refine_ls_hydrogen_treatment     none 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          12710 
_refine_ls_number_parameters      701 
_refine_ls_number_restraints      15 
_refine_ls_R_factor_all           0.1245 
_refine_ls_R_factor_gt            0.0506 
_refine_ls_wR_factor_ref          0.1337 
_refine_ls_wR_factor_gt           0.1171 
_refine_ls_goodness_of_fit_ref    0.925 
_refine_ls_restrained_S_all       0.932 
_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 
C201 C -0.002(3) 0.4979(17) 0.9744(12) 0.148(12) Uiso 0.50 1 d PD . 1 
C202 C -0.023(3) 0.5074(18) 0.9006(14) 0.220(17) Uiso 0.50 1 d PD A 1 
C203 C 0.024(5) 0.478(2) 0.8390(18) 0.41(4) Uiso 0.50 1 d PD A 1 
C204 C 0.045(3) 0.509(2) 0.7731(18) 0.26(2) Uiso 0.50 1 d PD A 1 
C101 C -0.035(3) 0.5054(19) 0.5426(15) 0.230(19) Uiso 0.50 1 d PD . 2 
C102 C 0.020(2) 0.4985(17) 0.6056(17) 0.192(14) Uiso 0.50 1 d PD B 2 
C103 C 0.015(3) 0.5049(19) 0.6806(18) 0.26(2) Uiso 0.50 1 d PD B 2 
C104 C 0.099(4) 0.474(3) 0.724(2) 0.36(3) Uiso 0.50 1 d PD B 2 
C302 C 0.1125(18) 0.2150(10) 0.7672(13) 0.324(12) Uiso 1 1 d D C 3 
C301 C 0.1487(16) 0.2838(10) 0.7466(14) 0.321(11) Uiso 1 1 d D C 3 
C303 C 0.1467(17) 0.1539(10) 0.7409(14) 0.317(11) Uiso 1 1 d D C 3 
C304 C 0.1461(15) 0.0826(10) 0.7566(15) 0.326(11) Uiso 1 1 d D C 3 
Si1 Si 0.32520(12) 0.42121(8) -0.05671(10) 0.0126(3) Uani 1 1 d . . . 
Si2 Si 0.17379(13) 0.31071(9) -0.03020(8) 0.0139(4) Uani 1 1 d . . . 
Si3 Si -0.04509(12) 0.27942(8) -0.06208(9) 0.0134(4) Uani 1 1 d . . . 
Si4 Si -0.03382(11) 0.12328(8) -0.06274(9) 0.0118(4) Uani 1 1 d . . . 
Si5 Si 0.17907(14) 0.07484(8) -0.02809(8) 0.0110(4) Uani 1 1 d . . . 
Si6 Si 0.31976(12) 0.19163(8) -0.05667(9) 0.0130(3) Uani 1 1 d . . . 
Si7 Si 0.32241(14) 0.42425(8) 0.17151(9) 0.0125(4) Uani 1 1 d . . . 
Si8 Si 0.17935(13) 0.30999(8) 0.12775(8) 0.0135(4) Uani 1 1 d . . . 
Si9 Si -0.03257(12) 0.27384(8) 0.17544(8) 0.0127(4) Uani 1 1 d . . . 
Si10 Si -0.03093(13) 0.12003(8) 0.17546(8) 0.0133(4) Uani 1 1 d . . . 
Si11 Si 0.17931(13) 0.07106(8) 0.12997(9) 0.0122(4) Uani 1 1 d . . . 
Si12 Si 0.31811(13) 0.18880(8) 0.16794(8) 0.0130(4) Uani 1 1 d . . . 
Si13 Si 0.33624(12) 0.42641(7) 0.55801(10) 0.0116(4) Uani 1 1 d . . . 
Si14 Si 0.19090(13) 0.31084(9) 0.52831(8) 0.0131(4) Uani 1 1 d . . . 
Si15 Si -0.02836(11) 0.27815(8) 0.56166(9) 0.0120(4) Uani 1 1 d . . . 
Si16 Si -0.03088(12) 0.12172(8) 0.56365(9) 0.0124(4) Uani 1 1 d . . . 
Si17 Si 0.18240(13) 0.07059(8) 0.52790(8) 0.0108(4) Uani 1 1 d . . . 
Si18 Si 0.32311(12) 0.18658(7) 0.56190(9) 0.0123(4) Uani 1 1 d . . . 
Si19 Si 0.31905(14) 0.42369(8) 0.32765(8) 0.0128(4) Uani 1 1 d . . . 
Si20 Si 0.17658(13) 0.31084(8) 0.36997(9) 0.0138(4) Uani 1 1 d . . . 
Si21 Si -0.03871(13) 0.27386(8) 0.33058(8) 0.0129(4) Uani 1 1 d . . . 
Si22 Si -0.03447(13) 0.11926(9) 0.32940(8) 0.0141(4) Uani 1 1 d . . . 
Si23 Si 0.17993(14) 0.07142(8) 0.36967(9) 0.0129(4) Uani 1 1 d . . . 
Si24 Si 0.30658(13) 0.19111(8) 0.32204(8) 0.0124(4) Uani 1 1 d . . . 
O1 O 0.2288(3) 0.3759(2) -0.0571(3) 0.0326(11) Uani 1 1 d . . . 
O2 O 0.0667(3) 0.30777(19) -0.0638(2) 0.0249(10) Uani 1 1 d . . . 
O3 O -0.0434(3) 0.20120(19) -0.0528(3) 0.0398(12) Uani 1 1 d . . . 
O4 O 0.0813(3) 0.1025(2) -0.0648(2) 0.0246(11) Uani 1 1 d . . . 
O5 O 0.2728(3) 0.1192(2) -0.0480(2) 0.0260(11) Uani 1 1 d . . . 
O6 O 0.2352(3) 0.2458(2) -0.0491(3) 0.0383(12) Uani 1 1 d . . . 
O7 O 0.2333(4) 0.3751(2) 0.1544(2) 0.0316(13) Uani 1 1 d . . . 
O8 O 0.0736(3) 0.3052(2) 0.1635(2) 0.0319(12) Uani 1 1 d . . . 
O9 O -0.0291(4) 0.1969(2) 0.15548(19) 0.0291(12) Uani 1 1 d . . . 
O10 O 0.0790(4) 0.0900(2) 0.1671(2) 0.0343(12) Uani 1 1 d . . . 
O11 O 0.2685(3) 0.1197(2) 0.1524(2) 0.0273(12) Uani 1 1 d . . . 
O12 O 0.2455(4) 0.2468(2) 0.1436(2) 0.0389(14) Uani 1 1 d . . . 
O13 O 0.1635(4) 0.3149(2) 0.0492(2) 0.0476(14) Uani 1 1 d . . . 
O14 O 0.1617(3) 0.0773(2) 0.0512(2) 0.0296(11) Uani 1 1 d . . . 
O15 O 0.3820(3) 0.4152(2) -0.1259(2) 0.0307(12) Uani 1 1 d . . . 
O16 O 0.3987(4) 0.3992(2) 0.0028(2) 0.0408(14) Uani 1 1 d . . . 
O17 O 0.4207(3) 0.4018(2) 0.1332(2) 0.0262(11) Uani 1 1 d . . . 
O18 O 0.3693(3) 0.1959(2) -0.1295(2) 0.0254(10) Uani 1 1 d . . . 
O19 O 0.4046(4) 0.2028(2) -0.0021(2) 0.0376(13) Uani 1 1 d . . . 
O20 O 0.4209(3) 0.1957(2) 0.1284(2) 0.0264(11) Uani 1 1 d . . . 
O21 O 0.2036(3) 0.00063(17) -0.0523(2) 0.0204(10) Uani 1 1 d . . . 
O22 O 0.2097(4) -0.0022(2) 0.1499(2) 0.0290(12) Uani 1 1 d . . . 
O23 O 0.3466(2) 0.42260(17) 0.2499(3) 0.0307(9) Uani 1 1 d . . . 
O24 O 0.3422(2) 0.19520(16) 0.2460(2) 0.0252(8) Uani 1 1 d . . . 
O25 O -0.0614(2) 0.28315(15) 0.2515(2) 0.0223(8) Uani 1 1 d . . . 
O26 O -0.0648(2) 0.11045(15) 0.2512(2) 0.0203(8) Uani 1 1 d . . . 
O27 O 0.2437(3) 0.3763(2) 0.5536(3) 0.0342(12) Uani 1 1 d . . . 
O28 O 0.0776(3) 0.31145(19) 0.5544(2) 0.0264(10) Uani 1 1 d . . . 
O29 O -0.0160(3) 0.1993(2) 0.5640(2) 0.0373(12) Uani 1 1 d . . . 
O30 O 0.0734(3) 0.0870(2) 0.5561(3) 0.0318(11) Uani 1 1 d . . . 
O31 O 0.2627(3) 0.1188(2) 0.5618(2) 0.0227(10) Uani 1 1 d . . . 
O32 O 0.2471(3) 0.2482(2) 0.5583(2) 0.0294(11) Uani 1 1 d . . . 
O33 O 0.2254(3) 0.3772(2) 0.3414(2) 0.0306(13) Uani 1 1 d . . . 
O34 O 0.0604(3) 0.3116(2) 0.35275(19) 0.0241(11) Uani 1 1 d . . . 
O35 O -0.0267(4) 0.19634(19) 0.34769(18) 0.0271(12) Uani 1 1 d . . . 
O36 O 0.0706(4) 0.0863(3) 0.3436(2) 0.0425(14) Uani 1 1 d . . . 
O37 O 0.2576(4) 0.1206(2) 0.3348(2) 0.0355(13) Uani 1 1 d . . . 
O38 O 0.2258(4) 0.2471(2) 0.3350(2) 0.0355(12) Uani 1 1 d . . . 
O39 O 0.1928(3) 0.3061(2) 0.4488(2) 0.0471(13) Uani 1 1 d . . . 
O40 O 0.1829(3) 0.0822(2) 0.4491(2) 0.0365(12) Uani 1 1 d . . . 
O41 O 0.3916(3) 0.4185(2) 0.6288(2) 0.0309(12) Uani 1 1 d . . . 
O42 O 0.4130(4) 0.4124(2) 0.4989(2) 0.0312(11) Uani 1 1 d . . . 
O43 O 0.4151(3) 0.3982(2) 0.3686(2) 0.0297(12) Uani 1 1 d . . . 
O44 O 0.3857(3) 0.1891(2) 0.6299(2) 0.0249(10) Uani 1 1 d . . . 
O45 O 0.3959(3) 0.1879(2) 0.4983(2) 0.0271(11) Uani 1 1 d . . . 
O46 O -0.0976(3) 0.2982(2) -0.1313(2) 0.0369(13) Uani 1 1 d . . . 
O47 O 0.2087(3) -0.00392(18) 0.5459(2) 0.0210(10) Uani 1 1 d . . . 
O48 O 0.2101(3) -0.0034(2) 0.3506(2) 0.0255(11) Uani 1 1 d . . . 
  
  
_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 
C201 C201 1.02(5) 3_567 ? 
C201 C202 1.510(18) . ? 
C202 C203 1.503(19) . ? 
C203 C204 1.480(19) . ? 
C101 C102 1.462(18) . ? 
C101 C101 1.95(6) 3_566 ? 
C102 C103 1.502(18) . ? 
C103 C104 1.546(19) . ? 
C302 C303 1.414(16) . ? 
C302 C301 1.525(16) . ? 
C303 C304 1.470(16) . ? 
Si1 O15 1.580(5) . ? 
Si1 O1 1.583(4) . ? 
Si1 O47 1.589(4) 2 ? 
Si1 O16 1.603(5) . ? 
Si2 O2 1.586(4) . ? 
Si2 O13 1.590(5) . ? 
Si2 O6 1.590(5) . ? 
Si2 O1 1.598(4) . ? 
Si3 O45 1.584(4) 4_565 ? 
Si3 O3 1.586(4) . ? 
Si3 O46 1.593(4) . ? 
Si3 O2 1.606(4) . ? 
Si4 O3 1.586(4) . ? 
Si4 O43 1.589(4) 4_565 ? 
Si4 O42 1.592(5) 4_565 ? 
Si4 O4 1.602(4) . ? 
Si5 O5 1.594(4) . ? 
Si5 O14 1.597(5) . ? 
Si5 O4 1.600(4) . ? 
Si5 O21 1.604(4) . ? 
Si6 O6 1.581(4) . ? 
Si6 O19 1.589(4) . ? 
Si6 O5 1.597(4) . ? 
Si6 O18 1.600(5) . ? 
Si7 O48 1.583(4) 2 ? 
Si7 O7 1.589(5) . ? 
Si7 O17 1.591(4) . ? 
Si7 O23 1.595(5) . ? 
Si8 O13 1.583(5) . ? 
Si8 O12 1.584(4) . ? 
Si8 O7 1.588(5) . ? 
Si8 O8 1.592(4) . ? 
Si9 O25 1.575(5) . ? 
Si9 O8 1.576(4) . ? 
Si9 O9 1.599(4) . ? 
Si9 O44 1.606(4) 4_565 ? 
Si10 O26 1.589(5) . ? 
Si10 O41 1.595(4) 4_565 ? 
Si10 O9 1.598(4) . ? 
Si10 O10 1.603(5) . ? 
Si11 O22 1.581(5) . ? 
Si11 O10 1.583(5) . ? 
Si11 O14 1.592(5) . ? 
Si11 O11 1.609(5) . ? 
Si12 O11 1.573(4) . ? 
Si12 O24 1.594(5) . ? 
Si12 O12 1.595(4) . ? 
Si12 O20 1.595(4) . ? 
Si13 O21 1.591(4) 2 ? 
Si13 O42 1.591(5) . ? 
Si13 O41 1.601(5) . ? 
Si13 O27 1.603(4) . ? 
Si14 O27 1.578(4) . ? 
Si14 O32 1.586(4) . ? 
Si14 O39 1.587(5) . ? 
Si14 O28 1.608(4) . ? 
Si15 O28 1.578(4) . ? 
Si15 O20 1.584(4) 4_566 ? 
Si15 O29 1.596(4) . ? 
Si15 O19 1.602(4) 4_566 ? 
Si16 O30 1.571(4) . ? 
Si16 O29 1.575(4) . ? 
Si16 O16 1.594(5) 4_566 ? 
Si16 O17 1.602(5) 4_566 ? 
Si17 O47 1.582(4) . ? 
Si17 O40 1.587(5) . ? 
Si17 O31 1.598(4) . ? 
Si17 O30 1.602(4) . ? 
Si18 O31 1.588(4) . ? 
Si18 O44 1.594(4) . ? 
Si18 O45 1.602(4) . ? 
Si18 O32 1.608(4) . ? 
Si19 O33 1.591(5) . ? 
Si19 O23 1.593(5) . ? 
Si19 O22 1.604(5) 2 ? 
Si19 O43 1.609(4) . ? 
Si20 O39 1.588(5) . ? 
Si20 O33 1.593(5) . ? 
Si20 O34 1.597(5) . ? 
Si20 O38 1.603(4) . ? 
Si21 O18 1.590(4) 4_566 ? 
Si21 O34 1.593(4) . ? 
Si21 O35 1.606(4) . ? 
Si21 O25 1.616(5) . ? 
Si22 O36 1.583(5) . ? 
Si22 O15 1.592(4) 4_566 ? 
Si22 O35 1.597(4) . ? 
Si22 O26 1.619(5) . ? 
Si23 O36 1.584(5) . ? 
Si23 O37 1.597(5) . ? 
Si23 O40 1.598(5) . ? 
Si23 O48 1.605(5) . ? 
Si24 O37 1.585(5) . ? 
Si24 O38 1.585(4) . ? 
Si24 O24 1.591(5) . ? 
Si24 O46 1.600(5) 4_666 ? 
O15 Si22 1.592(4) 4_665 ? 
O16 Si16 1.594(5) 4_665 ? 
O17 Si16 1.602(5) 4_665 ? 
O18 Si21 1.590(4) 4_665 ? 
O19 Si15 1.602(4) 4_665 ? 
O20 Si15 1.584(4) 4_665 ? 
O21 Si13 1.591(4) 2_545 ? 
O22 Si19 1.604(5) 2_545 ? 
O41 Si10 1.595(4) 4_666 ? 
O42 Si4 1.592(5) 4_666 ? 
O43 Si4 1.589(4) 4_666 ? 
O44 Si9 1.606(4) 4_666 ? 
O45 Si3 1.584(4) 4_666 ? 
O46 Si24 1.600(5) 4_565 ? 
O47 Si1 1.589(4) 2_545 ? 
O48 Si7 1.583(4) 2_545 ? 
  
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 
C201 C201 C202 166(6) 3_567 . ? 
C203 C202 C201 132(3) . . ? 
C204 C203 C202 130(4) . . ? 
C102 C101 C101 120(4) . 3_566 ? 
C101 C102 C103 145(3) . . ? 
C102 C103 C104 119(3) . . ? 
C303 C302 C301 126(2) . . ? 
C302 C303 C304 140(3) . . ? 
O15 Si1 O1 110.3(3) . . ? 
O15 Si1 O47 109.3(2) . 2 ? 
O1 Si1 O47 108.2(2) . 2 ? 
O15 Si1 O16 109.1(3) . . ? 
O1 Si1 O16 110.3(3) . . ? 
O47 Si1 O16 109.7(3) 2 . ? 
O2 Si2 O13 110.0(3) . . ? 
O2 Si2 O6 109.8(2) . . ? 
O13 Si2 O6 109.0(3) . . ? 
O2 Si2 O1 107.9(2) . . ? 
O13 Si2 O1 109.2(3) . . ? 
O6 Si2 O1 110.9(3) . . ? 
O45 Si3 O3 109.4(3) 4_565 . ? 
O45 Si3 O46 109.7(3) 4_565 . ? 
O3 Si3 O46 110.0(3) . . ? 
O45 Si3 O2 109.6(2) 4_565 . ? 
O3 Si3 O2 110.0(2) . . ? 
O46 Si3 O2 108.1(2) . . ? 
O3 Si4 O43 110.0(3) . 4_565 ? 
O3 Si4 O42 108.3(3) . 4_565 ? 
O43 Si4 O42 110.3(3) 4_565 4_565 ? 
O3 Si4 O4 109.9(2) . . ? 
O43 Si4 O4 108.8(3) 4_565 . ? 
O42 Si4 O4 109.6(3) 4_565 . ? 
O5 Si5 O14 110.2(2) . . ? 
O5 Si5 O4 109.8(2) . . ? 
O14 Si5 O4 108.7(2) . . ? 
O5 Si5 O21 106.6(2) . . ? 
O14 Si5 O21 110.9(2) . . ? 
O4 Si5 O21 110.7(2) . . ? 
O6 Si6 O19 110.5(3) . . ? 
O6 Si6 O5 109.7(3) . . ? 
O19 Si6 O5 109.7(3) . . ? 
O6 Si6 O18 110.4(3) . . ? 
O19 Si6 O18 108.4(3) . . ? 
O5 Si6 O18 108.2(3) . . ? 
O48 Si7 O7 107.9(3) 2 . ? 
O48 Si7 O17 110.9(3) 2 . ? 
O7 Si7 O17 110.1(3) . . ? 
O48 Si7 O23 110.3(2) 2 . ? 
O7 Si7 O23 110.5(2) . . ? 
O17 Si7 O23 107.2(2) . . ? 
O13 Si8 O12 108.8(2) . . ? 
O13 Si8 O7 109.8(3) . . ? 
O12 Si8 O7 109.9(3) . . ? 
O13 Si8 O8 109.1(3) . . ? 
O12 Si8 O8 111.3(3) . . ? 
O7 Si8 O8 107.9(3) . . ? 
O25 Si9 O8 108.7(2) . . ? 
O25 Si9 O9 111.2(2) . . ? 
O8 Si9 O9 108.9(3) . . ? 
O25 Si9 O44 108.7(2) . 4_565 ? 
O8 Si9 O44 110.2(3) . 4_565 ? 
O9 Si9 O44 109.2(2) . 4_565 ? 
O26 Si10 O41 107.9(2) . 4_565 ? 
O26 Si10 O9 111.0(2) . . ? 
O41 Si10 O9 109.7(2) 4_565 . ? 
O26 Si10 O10 108.5(2) . . ? 
O41 Si10 O10 110.8(3) 4_565 . ? 
O9 Si10 O10 109.0(3) . . ? 
O22 Si11 O10 109.1(3) . . ? 
O22 Si11 O14 111.0(2) . . ? 
O10 Si11 O14 108.4(3) . . ? 
O22 Si11 O11 107.8(3) . . ? 
O10 Si11 O11 110.9(3) . . ? 
O14 Si11 O11 109.6(2) . . ? 
O11 Si12 O24 110.4(2) . . ? 
O11 Si12 O12 109.2(3) . . ? 
O24 Si12 O12 111.2(2) . . ? 
O11 Si12 O20 110.2(2) . . ? 
O24 Si12 O20 107.5(2) . . ? 
O12 Si12 O20 108.3(2) . . ? 
O21 Si13 O42 109.3(3) 2 . ? 
O21 Si13 O41 108.1(2) 2 . ? 
O42 Si13 O41 109.5(3) . . ? 
O21 Si13 O27 109.1(2) 2 . ? 
O42 Si13 O27 110.5(3) . . ? 
O41 Si13 O27 110.2(3) . . ? 
O27 Si14 O32 109.3(3) . . ? 
O27 Si14 O39 111.1(3) . . ? 
O32 Si14 O39 108.7(3) . . ? 
O27 Si14 O28 108.3(2) . . ? 
O32 Si14 O28 109.5(2) . . ? 
O39 Si14 O28 109.9(3) . . ? 
O28 Si15 O20 108.9(3) . 4_566 ? 
O28 Si15 O29 109.3(2) . . ? 
O20 Si15 O29 110.5(3) 4_566 . ? 
O28 Si15 O19 109.3(3) . 4_566 ? 
O20 Si15 O19 110.1(2) 4_566 4_566 ? 
O29 Si15 O19 108.6(3) . 4_566 ? 
O30 Si16 O29 109.2(2) . . ? 
O30 Si16 O16 109.7(3) . 4_566 ? 
O29 Si16 O16 109.9(3) . 4_566 ? 
O30 Si16 O17 108.2(3) . 4_566 ? 
O29 Si16 O17 109.9(3) . 4_566 ? 
O16 Si16 O17 109.8(3) 4_566 4_566 ? 
O47 Si17 O40 111.2(2) . . ? 
O47 Si17 O31 109.2(2) . . ? 
O40 Si17 O31 109.0(2) . . ? 
O47 Si17 O30 108.6(2) . . ? 
O40 Si17 O30 108.7(3) . . ? 
O31 Si17 O30 110.0(3) . . ? 
O31 Si18 O44 107.4(2) . . ? 
O31 Si18 O45 108.9(2) . . ? 
O44 Si18 O45 110.5(2) . . ? 
O31 Si18 O32 109.8(2) . . ? 
O44 Si18 O32 110.3(3) . . ? 
O45 Si18 O32 109.9(2) . . ? 
O33 Si19 O23 110.1(2) . . ? 
O33 Si19 O22 108.0(3) . 2 ? 
O23 Si19 O22 109.9(2) . 2 ? 
O33 Si19 O43 111.0(3) . . ? 
O23 Si19 O43 107.6(2) . . ? 
O22 Si19 O43 110.3(3) 2 . ? 
O39 Si20 O33 110.3(3) . . ? 
O39 Si20 O34 110.3(2) . . ? 
O33 Si20 O34 108.5(2) . . ? 
O39 Si20 O38 109.0(3) . . ? 
O33 Si20 O38 110.3(3) . . ? 
O34 Si20 O38 108.5(2) . . ? 
O18 Si21 O34 109.1(2) 4_566 . ? 
O18 Si21 O35 110.1(3) 4_566 . ? 
O34 Si21 O35 108.7(2) . . ? 
O18 Si21 O25 107.3(2) 4_566 . ? 
O34 Si21 O25 111.8(2) . . ? 
O35 Si21 O25 109.8(2) . . ? 
O36 Si22 O15 110.2(3) . 4_566 ? 
O36 Si22 O35 107.9(3) . . ? 
O15 Si22 O35 110.0(3) 4_566 . ? 
O36 Si22 O26 110.5(2) . . ? 
O15 Si22 O26 108.3(2) 4_566 . ? 
O35 Si22 O26 110.0(2) . . ? 
O36 Si23 O37 110.1(3) . . ? 
O36 Si23 O40 108.7(3) . . ? 
O37 Si23 O40 109.4(3) . . ? 
O36 Si23 O48 109.5(3) . . ? 
O37 Si23 O48 108.3(3) . . ? 
O40 Si23 O48 110.8(2) . . ? 
O37 Si24 O38 109.0(3) . . ? 
O37 Si24 O24 108.9(2) . . ? 
O38 Si24 O24 108.9(2) . . ? 
O37 Si24 O46 111.2(3) . 4_666 ? 
O38 Si24 O46 111.0(3) . 4_666 ? 
O24 Si24 O46 107.7(2) . 4_666 ? 
Si1 O1 Si2 148.1(3) . . ? 
Si2 O2 Si3 148.3(3) . . ? 
Si3 O3 Si4 165.6(4) . . ? 
Si5 O4 Si4 150.4(3) . . ? 
Si5 O5 Si6 148.2(3) . . ? 
Si6 O6 Si2 164.1(4) . . ? 
Si8 O7 Si7 158.2(4) . . ? 
Si9 O8 Si8 153.9(3) . . ? 
Si10 O9 Si9 151.1(3) . . ? 
Si11 O10 Si10 157.3(3) . . ? 
Si12 O11 Si11 155.1(3) . . ? 
Si8 O12 Si12 172.1(3) . . ? 
Si8 O13 Si2 165.7(4) . . ? 
Si11 O14 Si5 162.0(3) . . ? 
Si1 O15 Si22 149.6(3) . 4_665 ? 
Si16 O16 Si1 178.1(4) 4_665 . ? 
Si7 O17 Si16 146.8(3) . 4_665 ? 
Si21 O18 Si6 142.9(3) 4_665 . ? 
Si6 O19 Si15 167.8(4) . 4_665 ? 
Si15 O20 Si12 144.7(3) 4_665 . ? 
Si13 O21 Si5 145.8(3) 2_545 . ? 
Si11 O22 Si19 151.1(3) . 2_545 ? 
Si19 O23 Si7 154.8(2) . . ? 
Si24 O24 Si12 149.8(2) . . ? 
Si9 O25 Si21 151.4(2) . . ? 
Si10 O26 Si22 146.0(2) . . ? 
Si14 O27 Si13 153.0(3) . . ? 
Si15 O28 Si14 151.5(3) . . ? 
Si16 O29 Si15 166.6(3) . . ? 
Si16 O30 Si17 159.8(3) . . ? 
Si18 O31 Si17 150.1(3) . . ? 
Si14 O32 Si18 158.7(3) . . ? 
Si19 O33 Si20 151.6(3) . . ? 
Si21 O34 Si20 150.4(3) . . ? 
Si22 O35 Si21 152.8(3) . . ? 
Si22 O36 Si23 164.2(4) . . ? 
Si24 O37 Si23 153.7(3) . . ? 
Si24 O38 Si20 157.2(3) . . ? 
Si14 O39 Si20 168.8(4) . . ? 
Si17 O40 Si23 163.7(3) . . ? 
Si10 O41 Si13 149.6(3) 4_666 . ? 
Si13 O42 Si4 160.4(4) . 4_666 ? 
Si4 O43 Si19 150.2(3) 4_666 . ? 
Si18 O44 Si9 148.7(3) . 4_666 ? 
Si3 O45 Si18 156.0(3) 4_666 . ? 
Si3 O46 Si24 152.8(3) . 4_565 ? 
Si17 O47 Si1 150.0(3) . 2_545 ? 
Si7 O48 Si23 149.3(3) 2_545 . ? 
  
_diffrn_measured_fraction_theta_max    0.840 
_diffrn_reflns_theta_full              29.58 
_diffrn_measured_fraction_theta_full   0.840 
_refine_diff_density_max    0.638 
_refine_diff_density_min   -0.823 
_refine_diff_density_rms    0.144 





  
data_f_hexane_twin_96 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C12 O48 Si24' 
_chemical_formula_weight          1586 
  
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' 
 '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' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    13.534(3) 
_cell_length_b                    20.319(5) 
_cell_length_c                    20.104(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.045(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      5528(2) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.18 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.836 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3080 
_exptl_absorpt_coefficient_mu     0.657 
_exptl_absorpt_correction_type    Analytical 
_exptl_absorpt_correction_T_min   0.8909 
_exptl_absorpt_correction_T_max   0.9567 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       296(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   'Bruker P4' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             59806 
_diffrn_reflns_av_R_equivalents   0.1521 
_diffrn_reflns_av_sigmaI/netI     0.0818 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        26 
_diffrn_reflns_limit_l_min        -26 
_diffrn_reflns_limit_l_max        26 
_diffrn_reflns_theta_min          1.00 
_diffrn_reflns_theta_max          27.68 
_reflns_number_total              12094 
_reflns_number_gt                 9106 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker XSCANS' 
_computing_cell_refinement        'Bruker XSCANS' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_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)+(0.0719P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none 
_refine_ls_hydrogen_treatment     none 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          12094 
_refine_ls_number_parameters      722 
_refine_ls_number_restraints      43 
_refine_ls_R_factor_all           0.0593 
_refine_ls_R_factor_gt            0.0455 
_refine_ls_wR_factor_ref          0.1449 
_refine_ls_wR_factor_gt           0.1362 
_refine_ls_goodness_of_fit_ref    1.003 
_refine_ls_restrained_S_all       1.024 
_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 
C201 C 0.507(3) 0.0172(17) 0.6108(13) 0.223(15) Uiso 0.50 1 d PDU . 1 
C202 C 0.541(3) 0.020(2) 0.5384(14) 0.36(3) Uiso 0.50 1 d PDU . 1 
C203 C 0.499(2) 0.0075(14) 0.4709(10) 0.160(10) Uiso 0.50 1 d PDU . 1 
C204 C 0.516(3) 0.024(2) 0.3996(11) 0.29(2) Uiso 0.50 1 d PDU . 1 
C205 C 0.4801(18) 0.0022(11) 0.3340(10) 0.147(9) Uiso 0.50 1 d PDU . 1 
C206 C 0.536(3) 0.000(2) 0.2704(16) 0.34(2) Uiso 0.50 1 d PDU A 1 
C101 C 0.480(3) -0.0154(17) -0.0709(9) 0.234(14) Uiso 0.50 1 d PDU . 2 
C102 C 0.5000 0.0000 0.0000 0.272(12) Uiso 1 2 d SDU . 2 
C103 C 0.508(4) -0.0408(16) 0.0602(10) 0.37(2) Uiso 0.50 1 d PDU . 2 
C104 C 0.461(2) -0.0020(16) 0.1156(11) 0.218(13) Uiso 0.50 1 d PDU . 2 
C105 C 0.5176(18) -0.0017(11) 0.1757(12) 0.171(10) Uiso 0.50 1 d PDU B 2 
C106 C 0.476(4) -0.005(3) 0.2440(16) 0.51(4) Uiso 0.50 1 d PDU B 2 
C301 C 0.2222(12) 0.0488(6) 0.7465(10) 0.270(7) Uiso 1 1 d DU C 3 
C302 C 0.1370(13) 0.0895(7) 0.7553(10) 0.268(7) Uiso 1 1 d DU C 3 
C303 C 0.1555(11) 0.1608(7) 0.7397(8) 0.253(6) Uiso 1 1 d DU C 3 
C304 C 0.1170(17) 0.2144(9) 0.7709(9) 0.340(10) Uiso 1 1 d DU C 3 
C305 C 0.1358(15) 0.2768(9) 0.7399(10) 0.299(8) Uiso 1 1 d DU C 3 
C306 C 0.1807(13) 0.3365(8) 0.7493(10) 0.287(8) Uiso 1 1 d DU C 3 
Si1 Si 0.32839(9) 0.42176(5) -0.05767(7) 0.0136(2) Uani 1 1 d . . . 
Si2 Si 0.17925(10) 0.30969(6) -0.03012(6) 0.0156(3) Uani 1 1 d . . . 
Si3 Si -0.04070(8) 0.27906(6) -0.06130(6) 0.0150(3) Uani 1 1 d . . . 
Si4 Si -0.03216(8) 0.12253(5) -0.06237(6) 0.0135(2) Uani 1 1 d . . . 
Si5 Si 0.18108(10) 0.07306(5) -0.02823(5) 0.0122(3) Uani 1 1 d . . . 
Si6 Si 0.32175(9) 0.18953(5) -0.05876(7) 0.0148(3) Uani 1 1 d . . . 
Si7 Si 0.32366(10) 0.42366(5) 0.17204(6) 0.0137(3) Uani 1 1 d . . . 
Si8 Si 0.18146(10) 0.30954(5) 0.12829(6) 0.0143(3) Uani 1 1 d . . . 
Si9 Si -0.03208(9) 0.27494(6) 0.17419(5) 0.0144(3) Uani 1 1 d . . . 
Si10 Si -0.02982(9) 0.12064(6) 0.17446(6) 0.0152(3) Uani 1 1 d . . . 
Si11 Si 0.18074(10) 0.07055(5) 0.13002(6) 0.0139(2) Uani 1 1 d . . . 
Si12 Si 0.31761(10) 0.18831(5) 0.17036(6) 0.0143(3) Uani 1 1 d . . . 
Si13 Si 0.33464(8) 0.42467(5) 0.55853(7) 0.0137(3) Uani 1 1 d . . . 
Si14 Si 0.18886(10) 0.30980(6) 0.52889(6) 0.0147(3) Uani 1 1 d . . . 
Si15 Si -0.03137(8) 0.27862(5) 0.56117(6) 0.0137(2) Uani 1 1 d . . . 
Si16 Si -0.03079(8) 0.12173(5) 0.56288(6) 0.0131(2) Uani 1 1 d . . . 
Si17 Si 0.18286(9) 0.07074(5) 0.52816(5) 0.0123(3) Uani 1 1 d . . . 
Si18 Si 0.32327(9) 0.18725(5) 0.56141(6) 0.0141(2) Uani 1 1 d . . . 
Si19 Si 0.32168(10) 0.42355(5) 0.32760(6) 0.0144(3) Uani 1 1 d . . . 
Si20 Si 0.18013(10) 0.30998(5) 0.37045(6) 0.0147(3) Uani 1 1 d . . . 
Si21 Si -0.03506(9) 0.27473(6) 0.32936(6) 0.0140(3) Uani 1 1 d . . . 
Si22 Si -0.03189(9) 0.12054(6) 0.32831(6) 0.0146(3) Uani 1 1 d . . . 
Si23 Si 0.18090(10) 0.07063(5) 0.36979(6) 0.0137(3) Uani 1 1 d . . . 
Si24 Si 0.31106(10) 0.18953(5) 0.32417(6) 0.0145(3) Uani 1 1 d . . . 
O1 O 0.2324(2) 0.37484(14) -0.05659(19) 0.0352(8) Uani 1 1 d . . . 
O2 O 0.0698(2) 0.30789(13) -0.06022(17) 0.0291(8) Uani 1 1 d . . . 
O3 O -0.0379(3) 0.20086(14) -0.0556(2) 0.0489(10) Uani 1 1 d . . . 
O4 O 0.0812(2) 0.09936(16) -0.06196(17) 0.0324(8) Uani 1 1 d . . . 
O5 O 0.2721(2) 0.11820(14) -0.05133(18) 0.0276(7) Uani 1 1 d . . . 
O6 O 0.2379(3) 0.24558(14) -0.0536(2) 0.0405(9) Uani 1 1 d . . . 
O7 O 0.2347(3) 0.37469(17) 0.15488(18) 0.0381(10) Uani 1 1 d . . . 
O8 O 0.0728(3) 0.30759(16) 0.15925(19) 0.0388(10) Uani 1 1 d . . . 
O9 O -0.0279(3) 0.19741(15) 0.15473(15) 0.0343(10) Uani 1 1 d . . . 
O10 O 0.0782(3) 0.09012(18) 0.16438(17) 0.0395(9) Uani 1 1 d . . . 
O11 O 0.2677(3) 0.11905(17) 0.15504(17) 0.0347(9) Uani 1 1 d . . . 
O12 O 0.2430(3) 0.24659(16) 0.15032(17) 0.0447(11) Uani 1 1 d . . . 
O13 O 0.1740(4) 0.31078(19) 0.04991(18) 0.0612(13) Uani 1 1 d . . . 
O14 O 0.1686(3) 0.07564(15) 0.05135(17) 0.0367(8) Uani 1 1 d . . . 
O15 O 0.3838(3) 0.41402(17) -0.12685(16) 0.0365(9) Uani 1 1 d . . . 
O16 O 0.4019(3) 0.40221(18) 0.00212(15) 0.0424(10) Uani 1 1 d . . . 
O17 O 0.4218(2) 0.40190(17) 0.13205(15) 0.0286(8) Uani 1 1 d . . . 
O18 O 0.3737(3) 0.19370(15) -0.12952(15) 0.0270(8) Uani 1 1 d . . . 
O19 O 0.4046(3) 0.19967(17) -0.00179(16) 0.0387(9) Uani 1 1 d . . . 
O20 O 0.4184(3) 0.19638(16) 0.12830(15) 0.0309(8) Uani 1 1 d . . . 
O21 O 0.2052(2) -0.00072(12) -0.05245(16) 0.0240(7) Uani 1 1 d . . . 
O22 O 0.2086(3) -0.00266(16) 0.15159(17) 0.0308(8) Uani 1 1 d . . . 
O23 O 0.34880(18) 0.42026(12) 0.24979(19) 0.0338(6) Uani 1 1 d . . . 
O24 O 0.34571(19) 0.19262(10) 0.24833(17) 0.0282(6) Uani 1 1 d . . . 
O25 O -0.05805(18) 0.28414(11) 0.25100(16) 0.0260(5) Uani 1 1 d . . . 
O26 O -0.06093(17) 0.11131(11) 0.25097(16) 0.0252(5) Uani 1 1 d . . . 
O27 O 0.2418(2) 0.37582(14) 0.5548(2) 0.0379(9) Uani 1 1 d . . . 
O28 O 0.0766(2) 0.31023(13) 0.55553(18) 0.0279(7) Uani 1 1 d . . . 
O29 O -0.0224(3) 0.19942(14) 0.5615(2) 0.0476(10) Uani 1 1 d . . . 
O30 O 0.0756(2) 0.09035(16) 0.55717(19) 0.0371(8) Uani 1 1 d . . . 
O31 O 0.2660(2) 0.11823(15) 0.55904(17) 0.0274(7) Uani 1 1 d . . . 
O32 O 0.2459(2) 0.24686(14) 0.55833(17) 0.0334(8) Uani 1 1 d . . . 
O33 O 0.2292(3) 0.37585(16) 0.34305(17) 0.0361(9) Uani 1 1 d . . . 
O34 O 0.0652(3) 0.31067(15) 0.34987(16) 0.0298(8) Uani 1 1 d . . . 
O35 O -0.0258(3) 0.19763(14) 0.34732(15) 0.0322(9) Uani 1 1 d . . . 
O36 O 0.0737(3) 0.08766(18) 0.34211(18) 0.0468(11) Uani 1 1 d . . . 
O37 O 0.2607(3) 0.11895(17) 0.33823(18) 0.0394(10) Uani 1 1 d . . . 
O38 O 0.2309(3) 0.24604(16) 0.33746(18) 0.0428(10) Uani 1 1 d . . . 
O39 O 0.1910(3) 0.30624(17) 0.44948(17) 0.0483(10) Uani 1 1 d . . . 
O40 O 0.1813(3) 0.07880(15) 0.44921(16) 0.0389(8) Uani 1 1 d . . . 
O41 O 0.3905(3) 0.41632(15) 0.62893(15) 0.0331(9) Uani 1 1 d . . . 
O42 O 0.4115(3) 0.41008(16) 0.49991(15) 0.0328(8) Uani 1 1 d . . . 
O43 O 0.4185(2) 0.39994(17) 0.36893(15) 0.0320(8) Uani 1 1 d . . . 
O44 O 0.3840(3) 0.19002(14) 0.63074(15) 0.0259(8) Uani 1 1 d . . . 
O45 O 0.3984(3) 0.19165(15) 0.49972(15) 0.0330(8) Uani 1 1 d . . . 
O46 O -0.0920(3) 0.30148(17) -0.12987(15) 0.0375(9) Uani 1 1 d . . . 
O47 O 0.2078(2) -0.00397(13) 0.54913(17) 0.0268(7) Uani 1 1 d . . . 
O48 O 0.2097(3) -0.00326(16) 0.34892(17) 0.0309(8) Uani 1 1 d . . . 
  
  
_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 
C201 C204 0.91(5) 3_656 ? 
C201 C205 1.19(3) 3_656 ? 
C201 C202 1.527(19) . ? 
C201 C203 1.72(4) 3_656 ? 
C202 C203 0.79(6) 3_656 ? 
C202 C203 1.491(18) . ? 
C202 C204 1.71(5) 3_656 ? 
C203 C202 0.79(6) 3_656 ? 
C203 C203 1.21(4) 3_656 ? 
C203 C204 1.490(17) . ? 
C203 C201 1.72(4) 3_656 ? 
C204 C201 0.91(5) 3_656 ? 
C204 C205 1.472(18) . ? 
C204 C202 1.71(5) 3_656 ? 
C205 C201 1.19(3) 3_656 ? 
C205 C206 1.486(19) . ? 
C101 C103 1.17(4) 3_655 ? 
C101 C104 1.25(4) 3_655 ? 
C101 C102 1.484(17) . ? 
C102 C103 1.470(18) . ? 
C102 C103 1.471(18) 3_655 ? 
C102 C101 1.484(17) 3_655 ? 
C103 C101 1.17(4) 3_655 ? 
C103 C104 1.508(19) . ? 
C104 C101 1.25(4) 3_655 ? 
C104 C105 1.430(18) . ? 
C105 C106 1.485(19) . ? 
C301 C302 1.430(14) . ? 
C302 C303 1.505(13) . ? 
C303 C304 1.361(15) . ? 
C304 C305 1.436(15) . ? 
C305 C306 1.369(15) . ? 
Si1 O15 1.589(3) . ? 
Si1 O47 1.596(3) 2 ? 
Si1 O16 1.609(3) . ? 
Si1 O1 1.612(3) . ? 
Si2 O6 1.597(3) . ? 
Si2 O1 1.598(3) . ? 
Si2 O2 1.600(3) . ? 
Si2 O13 1.611(4) . ? 
Si3 O45 1.594(3) 4_565 ? 
Si3 O3 1.594(3) . ? 
Si3 O2 1.606(3) . ? 
Si3 O46 1.608(3) . ? 
Si4 O3 1.599(3) . ? 
Si4 O43 1.600(3) 4_565 ? 
Si4 O4 1.605(3) . ? 
Si4 O42 1.610(3) 4_565 ? 
Si5 O4 1.603(3) . ? 
Si5 O5 1.604(3) . ? 
Si5 O21 1.610(3) . ? 
Si5 O14 1.610(4) . ? 
Si6 O18 1.589(3) . ? 
Si6 O5 1.605(3) . ? 
Si6 O6 1.611(3) . ? 
Si6 O19 1.615(3) . ? 
Si7 O7 1.600(3) . ? 
Si7 O23 1.601(4) . ? 
Si7 O48 1.608(3) 2 ? 
Si7 O17 1.615(3) . ? 
Si8 O13 1.579(4) . ? 
Si8 O12 1.589(3) . ? 
Si8 O8 1.598(4) . ? 
Si8 O7 1.599(3) . ? 
Si9 O25 1.595(3) . ? 
Si9 O8 1.595(4) . ? 
Si9 O44 1.600(3) 4_565 ? 
Si9 O9 1.624(3) . ? 
Si10 O41 1.600(3) 4_565 ? 
Si10 O10 1.601(4) . ? 
Si10 O26 1.606(3) . ? 
Si10 O9 1.610(3) . ? 
Si11 O14 1.593(3) . ? 
Si11 O22 1.595(3) . ? 
Si11 O10 1.601(4) . ? 
Si11 O11 1.615(3) . ? 
Si12 O11 1.591(3) . ? 
Si12 O12 1.607(3) . ? 
Si12 O20 1.613(4) . ? 
Si12 O24 1.615(4) . ? 
Si13 O42 1.600(3) . ? 
Si13 O27 1.603(3) . ? 
Si13 O41 1.613(3) . ? 
Si13 O21 1.613(3) 2 ? 
Si14 O39 1.598(4) . ? 
Si14 O32 1.607(3) . ? 
Si14 O27 1.607(3) . ? 
Si14 O28 1.611(3) . ? 
Si15 O20 1.595(3) 4_566 ? 
Si15 O19 1.595(3) 4_566 ? 
Si15 O28 1.600(3) . ? 
Si15 O29 1.614(3) . ? 
Si16 O30 1.579(3) . ? 
Si16 O29 1.583(3) . ? 
Si16 O16 1.599(3) 4_566 ? 
Si16 O17 1.605(3) 4_566 ? 
Si17 O40 1.596(3) . ? 
Si17 O31 1.607(3) . ? 
Si17 O47 1.611(3) . ? 
Si17 O30 1.614(3) . ? 
Si18 O32 1.602(3) . ? 
Si18 O31 1.603(3) . ? 
Si18 O45 1.607(3) . ? 
Si18 O44 1.618(3) . ? 
Si19 O23 1.608(4) . ? 
Si19 O22 1.610(3) 2 ? 
Si19 O33 1.613(3) . ? 
Si19 O43 1.623(3) . ? 
Si20 O33 1.593(3) . ? 
Si20 O39 1.597(4) . ? 
Si20 O34 1.609(4) . ? 
Si20 O38 1.612(3) . ? 
Si21 O34 1.595(3) . ? 
Si21 O35 1.612(3) . ? 
Si21 O25 1.617(3) . ? 
Si21 O18 1.619(3) 4_566 ? 
Si22 O36 1.601(4) . ? 
Si22 O35 1.614(3) . ? 
Si22 O26 1.615(3) . ? 
Si22 O15 1.615(3) 4_566 ? 
Si23 O37 1.592(4) . ? 
Si23 O36 1.592(4) . ? 
Si23 O40 1.605(3) . ? 
Si23 O48 1.607(3) . ? 
Si24 O24 1.597(4) . ? 
Si24 O38 1.602(4) . ? 
Si24 O37 1.613(4) . ? 
Si24 O46 1.615(4) 4_666 ? 
O15 Si22 1.615(3) 4_665 ? 
O16 Si16 1.599(3) 4_665 ? 
O17 Si16 1.605(3) 4_665 ? 
O18 Si21 1.619(3) 4_665 ? 
O19 Si15 1.595(3) 4_665 ? 
O20 Si15 1.595(3) 4_665 ? 
O21 Si13 1.614(3) 2_545 ? 
O22 Si19 1.610(3) 2_545 ? 
O41 Si10 1.600(3) 4_666 ? 
O42 Si4 1.610(3) 4_666 ? 
O43 Si4 1.600(3) 4_666 ? 
O44 Si9 1.600(3) 4_666 ? 
O45 Si3 1.594(3) 4_666 ? 
O46 Si24 1.615(4) 4_565 ? 
O47 Si1 1.596(3) 2_545 ? 
O48 Si7 1.608(3) 2_545 ? 
  
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 
C204 C201 C205 88(3) 3_656 3_656 ? 
C204 C201 C202 85(3) 3_656 . ? 
C205 C201 C202 149(4) 3_656 . ? 
C204 C201 C203 60(3) 3_656 3_656 ? 
C205 C201 C203 143(3) 3_656 3_656 ? 
C202 C201 C203 27(2) . 3_656 ? 
C203 C202 C203 54(3) 3_656 . ? 
C203 C202 C201 90(4) 3_656 . ? 
C203 C202 C201 138(3) . . ? 
C203 C202 C204 60(3) 3_656 3_656 ? 
C203 C202 C204 114(3) . 3_656 ? 
C201 C202 C204 32.1(19) . 3_656 ? 
C202 C203 C203 94(4) 3_656 3_656 ? 
C202 C203 C204 92(4) 3_656 . ? 
C203 C203 C204 170(5) 3_656 . ? 
C202 C203 C202 126(3) 3_656 . ? 
C203 C203 C202 32(3) 3_656 . ? 
C204 C203 C202 141(3) . . ? 
C202 C203 C201 63(3) 3_656 3_656 ? 
C203 C203 C201 149(4) 3_656 3_656 ? 
C204 C203 C201 32.1(19) . 3_656 ? 
C202 C203 C201 159(3) . 3_656 ? 
C201 C204 C205 54(2) 3_656 . ? 
C201 C204 C203 88(4) 3_656 . ? 
C205 C204 C203 138(3) . . ? 
C201 C204 C202 63(3) 3_656 3_656 ? 
C205 C204 C202 110(2) . 3_656 ? 
C203 C204 C202 28(2) . 3_656 ? 
C201 C205 C204 38(2) 3_656 . ? 
C201 C205 C206 136(4) 3_656 . ? 
C204 C205 C206 128(3) . . ? 
C103 C101 C104 77(3) 3_655 3_655 ? 
C103 C101 C102 66.0(14) 3_655 . ? 
C104 C101 C102 121(3) 3_655 . ? 
C103 C102 C103 179.996(4) . 3_655 ? 
C103 C102 C101 46.7(17) . 3_655 ? 
C103 C102 C101 133.3(17) 3_655 3_655 ? 
C103 C102 C101 133.3(17) . . ? 
C103 C102 C101 46.7(17) 3_655 . ? 
C101 C102 C101 180.0(4) 3_655 . ? 
C101 C103 C102 67.3(16) 3_655 . ? 
C101 C103 C104 54(2) 3_655 . ? 
C102 C103 C104 106(2) . . ? 
C101 C104 C105 105(3) 3_655 . ? 
C101 C104 C103 49(2) 3_655 . ? 
C105 C104 C103 114(2) . . ? 
C104 C105 C106 125(3) . . ? 
C301 C302 C303 113.4(14) . . ? 
C304 C303 C302 127.6(17) . . ? 
C303 C304 C305 115.9(19) . . ? 
C306 C305 C304 143(2) . . ? 
O15 Si1 O47 109.45(18) . 2 ? 
O15 Si1 O16 109.72(19) . . ? 
O47 Si1 O16 110.03(19) 2 . ? 
O15 Si1 O1 109.5(2) . . ? 
O47 Si1 O1 108.08(17) 2 . ? 
O16 Si1 O1 109.99(19) . . ? 
O6 Si2 O1 110.7(2) . . ? 
O6 Si2 O2 109.26(18) . . ? 
O1 Si2 O2 108.02(18) . . ? 
O6 Si2 O13 109.2(2) . . ? 
O1 Si2 O13 110.0(2) . . ? 
O2 Si2 O13 109.7(2) . . ? 
O45 Si3 O3 109.2(2) 4_565 . ? 
O45 Si3 O2 109.6(2) 4_565 . ? 
O3 Si3 O2 109.9(2) . . ? 
O45 Si3 O46 109.3(2) 4_565 . ? 
O3 Si3 O46 110.7(2) . . ? 
O2 Si3 O46 108.0(2) . . ? 
O3 Si4 O43 109.7(2) . 4_565 ? 
O3 Si4 O4 109.7(2) . . ? 
O43 Si4 O4 108.63(19) 4_565 . ? 
O3 Si4 O42 108.7(2) . 4_565 ? 
O43 Si4 O42 110.85(18) 4_565 4_565 ? 
O4 Si4 O42 109.21(19) . 4_565 ? 
O4 Si5 O5 109.50(17) . . ? 
O4 Si5 O21 110.69(18) . . ? 
O5 Si5 O21 106.81(17) . . ? 
O4 Si5 O14 108.70(19) . . ? 
O5 Si5 O14 110.49(19) . . ? 
O21 Si5 O14 110.63(17) . . ? 
O18 Si6 O5 108.48(18) . . ? 
O18 Si6 O6 109.4(2) . . ? 
O5 Si6 O6 109.71(18) . . ? 
O18 Si6 O19 108.7(2) . . ? 
O5 Si6 O19 109.87(19) . . ? 
O6 Si6 O19 110.7(2) . . ? 
O7 Si7 O23 110.06(18) . . ? 
O7 Si7 O48 107.84(19) . 2 ? 
O23 Si7 O48 110.80(16) . 2 ? 
O7 Si7 O17 109.99(18) . . ? 
O23 Si7 O17 107.46(16) . . ? 
O48 Si7 O17 110.69(19) 2 . ? 
O13 Si8 O12 108.9(2) . . ? 
O13 Si8 O8 109.3(2) . . ? 
O12 Si8 O8 110.7(2) . . ? 
O13 Si8 O7 110.4(2) . . ? 
O12 Si8 O7 109.7(2) . . ? 
O8 Si8 O7 107.7(2) . . ? 
O25 Si9 O8 109.29(18) . . ? 
O25 Si9 O44 108.64(16) . 4_565 ? 
O8 Si9 O44 110.1(2) . 4_565 ? 
O25 Si9 O9 110.77(15) . . ? 
O8 Si9 O9 109.1(2) . . ? 
O44 Si9 O9 108.95(19) 4_565 . ? 
O41 Si10 O10 111.1(2) 4_565 . ? 
O41 Si10 O26 108.38(16) 4_565 . ? 
O10 Si10 O26 108.40(17) . . ? 
O41 Si10 O9 108.94(19) 4_565 . ? 
O10 Si10 O9 109.2(2) . . ? 
O26 Si10 O9 110.77(15) . . ? 
O14 Si11 O22 110.77(17) . . ? 
O14 Si11 O10 108.9(2) . . ? 
O22 Si11 O10 108.62(19) . . ? 
O14 Si11 O11 110.11(19) . . ? 
O22 Si11 O11 108.2(2) . . ? 
O10 Si11 O11 110.2(2) . . ? 
O11 Si12 O12 109.7(2) . . ? 
O11 Si12 O20 110.31(19) . . ? 
O12 Si12 O20 108.94(19) . . ? 
O11 Si12 O24 109.60(16) . . ? 
O12 Si12 O24 110.53(17) . . ? 
O20 Si12 O24 107.75(17) . . ? 
O42 Si13 O27 111.14(19) . . ? 
O42 Si13 O41 108.79(19) . . ? 
O27 Si13 O41 110.1(2) . . ? 
O42 Si13 O21 109.60(18) . 2 ? 
O27 Si13 O21 108.46(17) . 2 ? 
O41 Si13 O21 108.76(17) . 2 ? 
O39 Si14 O32 108.83(19) . . ? 
O39 Si14 O27 110.7(2) . . ? 
O32 Si14 O27 109.3(2) . . ? 
O39 Si14 O28 110.5(2) . . ? 
O32 Si14 O28 109.57(18) . . ? 
O27 Si14 O28 107.94(17) . . ? 
O20 Si15 O19 110.57(19) 4_566 4_566 ? 
O20 Si15 O28 108.8(2) 4_566 . ? 
O19 Si15 O28 109.2(2) 4_566 . ? 
O20 Si15 O29 110.3(2) 4_566 . ? 
O19 Si15 O29 108.7(2) 4_566 . ? 
O28 Si15 O29 109.37(18) . . ? 
O30 Si16 O29 109.6(2) . . ? 
O30 Si16 O16 109.9(2) . 4_566 ? 
O29 Si16 O16 109.3(2) . 4_566 ? 
O30 Si16 O17 107.9(2) . 4_566 ? 
O29 Si16 O17 110.0(2) . 4_566 ? 
O16 Si16 O17 110.05(19) 4_566 4_566 ? 
O40 Si17 O31 109.37(19) . . ? 
O40 Si17 O47 111.07(17) . . ? 
O31 Si17 O47 108.56(18) . . ? 
O40 Si17 O30 108.8(2) . . ? 
O31 Si17 O30 109.98(19) . . ? 
O47 Si17 O30 109.03(18) . . ? 
O32 Si18 O31 110.14(19) . . ? 
O32 Si18 O45 110.01(18) . . ? 
O31 Si18 O45 109.39(18) . . ? 
O32 Si18 O44 109.78(18) . . ? 
O31 Si18 O44 107.52(17) . . ? 
O45 Si18 O44 110.0(2) . . ? 
O23 Si19 O22 110.48(16) . 2 ? 
O23 Si19 O33 109.87(17) . . ? 
O22 Si19 O33 108.16(19) 2 . ? 
O23 Si19 O43 107.52(16) . . ? 
O22 Si19 O43 110.35(19) 2 . ? 
O33 Si19 O43 110.46(18) . . ? 
O33 Si20 O39 110.22(19) . . ? 
O33 Si20 O34 107.89(19) . . ? 
O39 Si20 O34 110.2(2) . . ? 
O33 Si20 O38 110.9(2) . . ? 
O39 Si20 O38 109.4(2) . . ? 
O34 Si20 O38 108.3(2) . . ? 
O34 Si21 O35 108.7(2) . . ? 
O34 Si21 O25 111.15(17) . . ? 
O35 Si21 O25 110.37(15) . . ? 
O34 Si21 O18 109.63(17) . 4_566 ? 
O35 Si21 O18 109.26(19) . 4_566 ? 
O25 Si21 O18 107.71(15) . 4_566 ? 
O36 Si22 O35 108.6(2) . . ? 
O36 Si22 O26 109.57(18) . . ? 
O35 Si22 O26 110.68(15) . . ? 
O36 Si22 O15 110.6(2) . 4_566 ? 
O35 Si22 O15 109.02(19) . 4_566 ? 
O26 Si22 O15 108.38(16) . 4_566 ? 
O37 Si23 O36 110.2(2) . . ? 
O37 Si23 O40 109.33(19) . . ? 
O36 Si23 O40 109.1(2) . . ? 
O37 Si23 O48 107.90(19) . . ? 
O36 Si23 O48 109.5(2) . . ? 
O40 Si23 O48 110.83(17) . . ? 
O24 Si24 O38 109.29(18) . . ? 
O24 Si24 O37 109.07(16) . . ? 
O38 Si24 O37 108.8(2) . . ? 
O24 Si24 O46 107.62(18) . 4_666 ? 
O38 Si24 O46 111.94(19) . 4_666 ? 
O37 Si24 O46 110.1(2) . 4_666 ? 
Si2 O1 Si1 149.0(2) . . ? 
Si2 O2 Si3 151.1(2) . . ? 
Si3 O3 Si4 170.9(3) . . ? 
Si5 O4 Si4 154.9(2) . . ? 
Si5 O5 Si6 149.9(2) . . ? 
Si2 O6 Si6 161.1(3) . . ? 
Si8 O7 Si7 157.8(3) . . ? 
Si9 O8 Si8 154.5(2) . . ? 
Si10 O9 Si9 151.6(2) . . ? 
Si10 O10 Si11 160.5(3) . . ? 
Si12 O11 Si11 155.4(3) . . ? 
Si8 O12 Si12 172.7(3) . . ? 
Si8 O13 Si2 173.6(3) . . ? 
Si11 O14 Si5 166.8(3) . . ? 
Si1 O15 Si22 150.0(2) . 4_665 ? 
Si16 O16 Si1 175.6(3) 4_665 . ? 
Si16 O17 Si7 147.4(2) 4_665 . ? 
Si6 O18 Si21 144.7(2) . 4_665 ? 
Si15 O19 Si6 166.9(3) 4_665 . ? 
Si15 O20 Si12 146.8(2) 4_665 . ? 
Si5 O21 Si13 146.1(2) . 2_545 ? 
Si11 O22 Si19 151.5(3) . 2_545 ? 
Si7 O23 Si19 154.07(18) . . ? 
Si24 O24 Si12 148.82(18) . . ? 
Si9 O25 Si21 152.50(16) . . ? 
Si10 O26 Si22 147.65(16) . . ? 
Si13 O27 Si14 151.8(2) . . ? 
Si15 O28 Si14 152.0(2) . . ? 
Si16 O29 Si15 171.5(3) . . ? 
Si16 O30 Si17 161.1(3) . . ? 
Si18 O31 Si17 151.1(2) . . ? 
Si18 O32 Si14 158.4(2) . . ? 
Si20 O33 Si19 153.6(3) . . ? 
Si21 O34 Si20 152.2(2) . . ? 
Si21 O35 Si22 152.3(2) . . ? 
Si23 O36 Si22 164.6(3) . . ? 
Si23 O37 Si24 154.9(3) . . ? 
Si24 O38 Si20 159.2(3) . . ? 
Si20 O39 Si14 171.7(3) . . ? 
Si17 O40 Si23 168.2(2) . . ? 
Si10 O41 Si13 150.0(2) 4_666 . ? 
Si13 O42 Si4 163.4(3) . 4_666 ? 
Si4 O43 Si19 149.6(2) 4_666 . ? 
Si9 O44 Si18 147.7(2) 4_666 . ? 
Si3 O45 Si18 160.5(2) 4_666 . ? 
Si3 O46 Si24 150.7(3) . 4_565 ? 
Si1 O47 Si17 148.8(2) 2_545 . ? 
Si23 O48 Si7 149.6(3) . 2_545 ? 
  
_diffrn_measured_fraction_theta_max    0.934 
_diffrn_reflns_theta_full              27.68 
_diffrn_measured_fraction_theta_full   0.934 
_refine_diff_density_max    0.805 
_refine_diff_density_min   -0.678 
_refine_diff_density_rms    0.108 



  
data_f_pentane_6h_twin 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C10 O48 Si24' 
_chemical_formula_weight          1562 
  
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' 
 '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' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    13.47(2) 
_cell_length_b                    20.190(10) 
_cell_length_c                    19.980(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.020(7) 
_cell_angle_gamma                 90.00 
_cell_volume                      5434(9) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.13 
_exptl_crystal_size_mid           0.09 
_exptl_crystal_size_min           0.05 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.851 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3048 
_exptl_absorpt_coefficient_mu     0.667 
_exptl_absorpt_correction_type    Analytical 
_exptl_absorpt_correction_T_min   0.9200 
_exptl_absorpt_correction_T_max   0.9661 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       296(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   'Bruker P4' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             63363 
_diffrn_reflns_av_R_equivalents   0.1096 
_diffrn_reflns_av_sigmaI/netI     0.1329 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        26 
_diffrn_reflns_limit_l_min        -25 
_diffrn_reflns_limit_l_max        25 
_diffrn_reflns_theta_min          1.01 
_diffrn_reflns_theta_max          28.65 
_reflns_number_total              13092 
_reflns_number_gt                 5585 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker XSCANS' 
_computing_cell_refinement        'Bruker XSCANS' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_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)+(0.0445P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none
_refine_ls_hydrogen_treatment     none 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          13092 
_refine_ls_number_parameters      713 
_refine_ls_number_restraints      21 
_refine_ls_R_factor_all           0.1371 
_refine_ls_R_factor_gt            0.0492 
_refine_ls_wR_factor_ref          0.1281 
_refine_ls_wR_factor_gt           0.1060 
_refine_ls_goodness_of_fit_ref    0.820 
_refine_ls_restrained_S_all       0.823 
_refine_ls_shift/su_max           0.002 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
C101 C 0.482(4) 0.996(3) -0.0681(18) 0.22(2) Uiso 0.50 1 d PD . 1 
C105 C 0.485(4) 0.997(2) 0.1980(16) 0.210(19) Uiso 0.50 1 d PD A 1 
C104 C 0.517(2) 1.0067(16) 0.1281(15) 0.134(12) Uiso 0.50 1 d PD . 1 
C103 C 0.468(4) 0.976(3) 0.0678(18) 0.23(3) Uiso 0.50 1 d PD . 1 
C102 C 0.484(8) 1.018(3) 0.0050(19) 0.34(4) Uiso 0.50 1 d PD . 1 
C201 C 0.504(3) 0.9983(18) 0.4714(12) 0.123(12) Uiso 0.50 1 d PD . 2 
C203 C 0.517(3) 0.985(2) 0.3450(15) 0.22(2) Uiso 0.50 1 d PD B 2 
C204 C 0.518(5) 1.030(2) 0.285(2) 0.31(3) Uiso 0.50 1 d PD B 2 
C202 C 0.462(3) 1.0117(19) 0.4036(15) 0.184(17) Uiso 0.50 1 d PD B 2 
C205 C 0.571(5) 1.004(3) 0.223(2) 0.40(4) Uiso 0.50 1 d PD B 2 
C301 C 0.1604(14) 0.3084(9) 0.7473(19) 0.263(9) Uiso 1 1 d D C 3 
C302 C 0.1188(15) 0.2421(9) 0.7600(15) 0.246(9) Uiso 1 1 d D C 3 
C303 C 0.1490(13) 0.1786(9) 0.7359(12) 0.222(9) Uiso 1 1 d D C 3 
C304 C 0.1278(14) 0.1096(9) 0.7569(16) 0.232(9) Uiso 1 1 d D C 3 
C305 C 0.2015(17) 0.0564(10) 0.747(3) 0.354(14) Uiso 1 1 d D C 3 
Si1 Si 0.32540(17) 0.42110(11) -0.05700(14) 0.0145(5) Uani 1 1 d . . . 
Si2 Si 0.17399(18) 0.31078(13) -0.03022(11) 0.0164(5) Uani 1 1 d . . . 
Si3 Si -0.04480(17) 0.27914(11) -0.06196(14) 0.0169(5) Uani 1 1 d . . . 
Si4 Si -0.03410(16) 0.12312(11) -0.06253(13) 0.0138(5) Uani 1 1 d . . . 
Si5 Si 0.17897(19) 0.07465(11) -0.02797(11) 0.0135(5) Uani 1 1 d . . . 
Si6 Si 0.31979(17) 0.19193(11) -0.05689(13) 0.0159(5) Uani 1 1 d . . . 
Si7 Si 0.32234(19) 0.42431(12) 0.17141(12) 0.0145(5) Uani 1 1 d . . . 
Si8 Si 0.17906(17) 0.31027(12) 0.12753(12) 0.0151(5) Uani 1 1 d . . . 
Si9 Si -0.03300(18) 0.27419(12) 0.17489(12) 0.0154(6) Uani 1 1 d . . . 
Si10 Si -0.03105(18) 0.12008(12) 0.17526(12) 0.0158(6) Uani 1 1 d . . . 
Si11 Si 0.17919(19) 0.07120(11) 0.12998(13) 0.0149(5) Uani 1 1 d . . . 
Si12 Si 0.31725(18) 0.18916(13) 0.16837(12) 0.0160(5) Uani 1 1 d . . . 
Si13 Si 0.33560(17) 0.42641(10) 0.55814(15) 0.0140(5) Uani 1 1 d . . . 
Si14 Si 0.18992(18) 0.31104(13) 0.52833(11) 0.0159(5) Uani 1 1 d . . . 
Si15 Si -0.02944(16) 0.27813(11) 0.56119(13) 0.0145(5) Uani 1 1 d . . . 
Si16 Si -0.03138(17) 0.12162(11) 0.56295(14) 0.0150(5) Uani 1 1 d . . . 
Si17 Si 0.18164(19) 0.07070(11) 0.52750(12) 0.0142(5) Uani 1 1 d . . . 
Si18 Si 0.32220(17) 0.18665(11) 0.56207(13) 0.0144(5) Uani 1 1 d . . . 
Si19 Si 0.31936(19) 0.42374(12) 0.32734(13) 0.0157(6) Uani 1 1 d . . . 
Si20 Si 0.17689(18) 0.31069(12) 0.36991(12) 0.0158(5) Uani 1 1 d . . . 
Si21 Si -0.03840(18) 0.27424(12) 0.33029(12) 0.0149(6) Uani 1 1 d . . . 
Si22 Si -0.03423(19) 0.11968(12) 0.32902(12) 0.0163(6) Uani 1 1 d . . . 
Si23 Si 0.17947(19) 0.07119(11) 0.36943(13) 0.0142(5) Uani 1 1 d . . . 
Si24 Si 0.30686(18) 0.19101(12) 0.32244(11) 0.0153(5) Uani 1 1 d . . . 
O1 O 0.2285(4) 0.3754(3) -0.0576(4) 0.0342(16) Uani 1 1 d . . . 
O2 O 0.0646(4) 0.3078(3) -0.0633(3) 0.0258(14) Uani 1 1 d . . . 
O3 O -0.0438(5) 0.2014(3) -0.0524(4) 0.0431(16) Uani 1 1 d . . . 
O4 O 0.0802(4) 0.1019(3) -0.0647(3) 0.0251(14) Uani 1 1 d . . . 
O5 O 0.2723(4) 0.1197(3) -0.0482(3) 0.0252(15) Uani 1 1 d . . . 
O6 O 0.2348(4) 0.2459(3) -0.0506(4) 0.0398(17) Uani 1 1 d . . . 
O7 O 0.2334(5) 0.3759(3) 0.1545(3) 0.0328(19) Uani 1 1 d . . . 
O8 O 0.0733(4) 0.3050(3) 0.1625(3) 0.0347(16) Uani 1 1 d . . . 
O9 O -0.0296(5) 0.1969(3) 0.1554(3) 0.0322(17) Uani 1 1 d . . . 
O10 O 0.0775(5) 0.0901(3) 0.1660(3) 0.0349(17) Uani 1 1 d . . . 
O11 O 0.2674(5) 0.1198(3) 0.1529(3) 0.0302(17) Uani 1 1 d . . . 
O12 O 0.2443(5) 0.2467(3) 0.1438(3) 0.0385(18) Uani 1 1 d . . . 
O13 O 0.1665(5) 0.3140(3) 0.0492(3) 0.0507(19) Uani 1 1 d . . . 
O14 O 0.1622(4) 0.0771(3) 0.0513(3) 0.0328(15) Uani 1 1 d . . . 
O15 O 0.3819(5) 0.4139(3) -0.1256(3) 0.0313(17) Uani 1 1 d . . . 
O16 O 0.3973(5) 0.3985(4) 0.0029(3) 0.047(2) Uani 1 1 d . . . 
O17 O 0.4191(5) 0.4014(3) 0.1317(3) 0.0281(16) Uani 1 1 d . . . 
O18 O 0.3701(4) 0.1959(3) -0.1294(3) 0.0287(15) Uani 1 1 d . . . 
O19 O 0.4045(5) 0.2031(3) -0.0020(3) 0.0385(18) Uani 1 1 d . . . 
O20 O 0.4190(4) 0.1957(3) 0.1276(3) 0.0267(14) Uani 1 1 d . . . 
O21 O 0.2041(4) 0.0011(2) -0.0530(3) 0.0222(14) Uani 1 1 d . . . 
O22 O 0.2080(5) -0.0028(3) 0.1502(3) 0.0314(17) Uani 1 1 d . . . 
O23 O 0.3469(3) 0.4214(2) 0.2504(4) 0.0306(11) Uani 1 1 d . . . 
O24 O 0.3436(3) 0.1950(2) 0.2457(3) 0.0259(10) Uani 1 1 d . . . 
O25 O -0.0608(3) 0.28386(18) 0.2518(3) 0.0243(10) Uani 1 1 d . . . 
O26 O -0.0640(3) 0.11072(18) 0.2515(4) 0.0224(10) Uani 1 1 d . . . 
O27 O 0.2430(4) 0.3765(3) 0.5534(4) 0.0330(16) Uani 1 1 d . . . 
O28 O 0.0776(4) 0.3121(2) 0.5547(3) 0.0258(13) Uani 1 1 d . . . 
O29 O -0.0160(4) 0.1999(3) 0.5645(3) 0.0403(17) Uani 1 1 d . . . 
O30 O 0.0715(4) 0.0861(3) 0.5542(4) 0.0345(16) Uani 1 1 d . . . 
O31 O 0.2613(4) 0.1191(3) 0.5621(3) 0.0270(15) Uani 1 1 d . . . 
O32 O 0.2464(4) 0.2484(3) 0.5581(3) 0.0321(15) Uani 1 1 d . . . 
O33 O 0.2261(5) 0.3769(3) 0.3419(3) 0.0304(18) Uani 1 1 d . . . 
O34 O 0.0606(4) 0.3121(3) 0.3525(3) 0.0264(15) Uani 1 1 d . . . 
O35 O -0.0255(5) 0.1970(3) 0.3476(3) 0.0290(16) Uani 1 1 d . . . 
O36 O 0.0709(5) 0.0858(3) 0.3428(3) 0.043(2) Uani 1 1 d . . . 
O37 O 0.2575(5) 0.1204(3) 0.3356(3) 0.0375(19) Uani 1 1 d . . . 
O38 O 0.2260(5) 0.2472(3) 0.3342(3) 0.0363(17) Uani 1 1 d . . . 
O39 O 0.1932(4) 0.3063(3) 0.4487(3) 0.0471(17) Uani 1 1 d . . . 
O40 O 0.1831(4) 0.0809(3) 0.4492(3) 0.0355(15) Uani 1 1 d . . . 
O41 O 0.3909(5) 0.4188(3) 0.6290(3) 0.0323(17) Uani 1 1 d . . . 
O42 O 0.4115(5) 0.4116(3) 0.4985(3) 0.0299(15) Uani 1 1 d . . . 
O43 O 0.4161(4) 0.3988(3) 0.3684(3) 0.0283(16) Uani 1 1 d . . . 
O44 O 0.3842(4) 0.1893(3) 0.6303(3) 0.0247(14) Uani 1 1 d . . . 
O45 O 0.3958(4) 0.1889(3) 0.4985(3) 0.0268(14) Uani 1 1 d . . . 
O46 O -0.0971(4) 0.2978(3) -0.1304(3) 0.0388(18) Uani 1 1 d . . . 
O47 O 0.2084(4) -0.0046(3) 0.5463(3) 0.0241(15) Uani 1 1 d . . . 
O48 O 0.2111(5) -0.0023(3) 0.3498(3) 0.0283(17) Uani 1 1 d . . . 
  
  
_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 
C101 C103 0.87(8) 3_675 ? 
C101 C104 1.20(5) 3_675 ? 
C101 C102 1.37(7) 3_675 ? 
C101 C102 1.53(2) . ? 
C105 C104 1.470(18) . ? 
C104 C101 1.20(5) 3_675 ? 
C104 C103 1.498(19) . ? 
C103 C101 0.87(8) 3_675 ? 
C103 C102 1.52(2) . ? 
C103 C102 1.60(9) 3_675 ? 
C102 C102 0.88(15) 3_675 ? 
C102 C101 1.37(7) 3_675 ? 
C102 C103 1.60(9) 3_675 ? 
C201 C201 1.15(5) 3_676 ? 
C201 C202 1.494(19) . ? 
C203 C202 1.488(19) . ? 
C203 C204 1.491(19) . ? 
C204 C205 1.53(2) . ? 
C301 C302 1.472(15) . ? 
C302 C303 1.430(15) . ? 
C303 C304 1.483(15) . ? 
C304 C305 1.476(16) . ? 
Si1 O15 1.575(7) . ? 
Si1 O47 1.583(6) 2 ? 
Si1 O1 1.598(6) . ? 
Si1 O16 1.606(7) . ? 
Si2 O13 1.592(7) . ? 
Si2 O1 1.594(6) . ? 
Si2 O6 1.598(6) . ? 
Si2 O2 1.615(6) . ? 
Si3 O3 1.580(6) . ? 
Si3 O46 1.584(6) . ? 
Si3 O2 1.584(6) . ? 
Si3 O45 1.586(6) 4_565 ? 
Si4 O42 1.586(6) 4_565 ? 
Si4 O43 1.597(6) 4_565 ? 
Si4 O4 1.599(6) . ? 
Si4 O3 1.599(6) . ? 
Si5 O14 1.601(7) . ? 
Si5 O5 1.604(6) . ? 
Si5 O21 1.604(5) . ? 
Si5 O4 1.615(6) . ? 
Si6 O6 1.585(6) . ? 
Si6 O19 1.599(6) . ? 
Si6 O18 1.601(6) . ? 
Si6 O5 1.602(6) . ? 
Si7 O7 1.582(7) . ? 
Si7 O17 1.594(7) . ? 
Si7 O48 1.605(6) 2 ? 
Si7 O23 1.613(8) . ? 
Si8 O13 1.575(7) . ? 
Si8 O12 1.588(6) . ? 
Si8 O8 1.590(6) . ? 
Si8 O7 1.607(6) . ? 
Si9 O8 1.582(6) . ? 
Si9 O25 1.594(7) . ? 
Si9 O44 1.607(6) 4_565 ? 
Si9 O9 1.608(6) . ? 
Si10 O10 1.593(7) . ? 
Si10 O26 1.598(7) . ? 
Si10 O9 1.602(6) . ? 
Si10 O41 1.605(6) 4_565 ? 
Si11 O14 1.593(7) . ? 
Si11 O10 1.594(7) . ? 
Si11 O22 1.595(7) . ? 
Si11 O11 1.608(6) . ? 
Si12 O11 1.583(6) . ? 
Si12 O24 1.590(7) . ? 
Si12 O12 1.600(6) . ? 
Si12 O20 1.600(6) . ? 
Si13 O42 1.598(7) . ? 
Si13 O21 1.602(5) 2 ? 
Si13 O27 1.606(6) . ? 
Si13 O41 1.607(7) . ? 
Si14 O27 1.584(6) . ? 
Si14 O32 1.591(6) . ? 
Si14 O39 1.594(6) . ? 
Si14 O28 1.602(6) . ? 
Si15 O20 1.588(6) 4_566 ? 
Si15 O19 1.589(6) 4_566 ? 
Si15 O29 1.591(6) . ? 
Si15 O28 1.602(6) . ? 
Si16 O30 1.570(6) . ? 
Si16 O16 1.590(7) 4_566 ? 
Si16 O29 1.595(6) . ? 
Si16 O17 1.597(7) 4_566 ? 
Si17 O40 1.578(7) . ? 
Si17 O47 1.606(6) . ? 
Si17 O30 1.608(6) . ? 
Si17 O31 1.608(6) . ? 
Si18 O31 1.592(6) . ? 
Si18 O44 1.599(6) . ? 
Si18 O45 1.612(6) . ? 
Si18 O32 1.613(6) . ? 
Si19 O23 1.583(7) . ? 
Si19 O22 1.593(7) 2 ? 
Si19 O33 1.599(7) . ? 
Si19 O43 1.620(6) . ? 
Si20 O39 1.592(6) . ? 
Si20 O33 1.594(6) . ? 
Si20 O34 1.605(6) . ? 
Si20 O38 1.609(6) . ? 
Si21 O18 1.592(6) 4_566 ? 
Si21 O34 1.599(6) . ? 
Si21 O35 1.607(6) . ? 
Si21 O25 1.609(7) . ? 
Si22 O36 1.596(7) . ? 
Si22 O15 1.599(6) 4_566 ? 
Si22 O35 1.609(6) . ? 
Si22 O26 1.609(7) . ? 
Si23 O36 1.583(7) . ? 
Si23 O48 1.593(6) . ? 
Si23 O37 1.596(7) . ? 
Si23 O40 1.607(7) . ? 
Si24 O38 1.591(6) . ? 
Si24 O37 1.595(7) . ? 
Si24 O24 1.613(7) . ? 
Si24 O46 1.616(6) 4_666 ? 
O15 Si22 1.599(6) 4_665 ? 
O16 Si16 1.590(7) 4_665 ? 
O17 Si16 1.597(7) 4_665 ? 
O18 Si21 1.592(6) 4_665 ? 
O19 Si15 1.589(6) 4_665 ? 
O20 Si15 1.588(6) 4_665 ? 
O21 Si13 1.602(5) 2_545 ? 
O22 Si19 1.593(7) 2_545 ? 
O41 Si10 1.605(6) 4_666 ? 
O42 Si4 1.586(6) 4_666 ? 
O43 Si4 1.597(6) 4_666 ? 
O44 Si9 1.607(6) 4_666 ? 
O45 Si3 1.586(6) 4_666 ? 
O46 Si24 1.616(6) 4_565 ? 
O47 Si1 1.583(6) 2_545 ? 
O48 Si7 1.605(6) 2_545 ? 
  
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 
C103 C101 C104 91(5) 3_675 3_675 ? 
C103 C101 C102 82(5) 3_675 3_675 ? 
C104 C101 C102 155(7) 3_675 3_675 ? 
C103 C101 C102 78(6) 3_675 . ? 
C104 C101 C102 165(5) 3_675 . ? 
C102 C101 C102 35(6) 3_675 . ? 
C101 C104 C105 161(5) 3_675 . ? 
C101 C104 C103 36(4) 3_675 . ? 
C105 C104 C103 126(3) . . ? 
C101 C103 C104 53(4) 3_675 . ? 
C101 C103 C102 63(5) 3_675 . ? 
C104 C103 C102 112(3) . . ? 
C101 C103 C102 70(6) 3_675 3_675 ? 
C104 C103 C102 122(5) . 3_675 ? 
C102 C103 C102 32(5) . 3_675 ? 
C102 C102 C101 83(7) 3_675 3_675 ? 
C102 C102 C103 78(6) 3_675 . ? 
C101 C102 C103 35(3) 3_675 . ? 
C102 C102 C101 63(5) 3_675 . ? 
C101 C102 C101 145(6) 3_675 . ? 
C103 C102 C101 128(3) . . ? 
C102 C102 C103 69(6) 3_675 3_675 ? 
C101 C102 C103 136(9) 3_675 3_675 ? 
C103 C102 C103 148(5) . 3_675 ? 
C101 C102 C103 32(3) . 3_675 ? 
C201 C201 C202 148(5) 3_676 . ? 
C202 C203 C204 115(3) . . ? 
C203 C204 C205 117(3) . . ? 
C203 C202 C201 117(3) . . ? 
C303 C302 C301 130(2) . . ? 
C302 C303 C304 134(2) . . ? 
C305 C304 C303 121(2) . . ? 
O15 Si1 O47 110.2(4) . 2 ? 
O15 Si1 O1 109.6(4) . . ? 
O47 Si1 O1 108.3(3) 2 . ? 
O15 Si1 O16 109.3(4) . . ? 
O47 Si1 O16 110.0(4) 2 . ? 
O1 Si1 O16 109.5(4) . . ? 
O13 Si2 O1 109.8(4) . . ? 
O13 Si2 O6 108.7(4) . . ? 
O1 Si2 O6 110.4(4) . . ? 
O13 Si2 O2 110.6(3) . . ? 
O1 Si2 O2 108.0(3) . . ? 
O6 Si2 O2 109.4(3) . . ? 
O3 Si3 O46 110.1(4) . . ? 
O3 Si3 O2 110.9(3) . . ? 
O46 Si3 O2 108.2(4) . . ? 
O3 Si3 O45 108.4(4) . 4_565 ? 
O46 Si3 O45 109.7(4) . 4_565 ? 
O2 Si3 O45 109.5(3) . 4_565 ? 
O42 Si4 O43 110.4(3) 4_565 4_565 ? 
O42 Si4 O4 110.4(4) 4_565 . ? 
O43 Si4 O4 107.9(4) 4_565 . ? 
O42 Si4 O3 107.6(4) 4_565 . ? 
O43 Si4 O3 110.4(4) 4_565 . ? 
O4 Si4 O3 110.3(3) . . ? 
O14 Si5 O5 110.0(3) . . ? 
O14 Si5 O21 111.6(3) . . ? 
O5 Si5 O21 106.3(3) . . ? 
O14 Si5 O4 108.8(3) . . ? 
O5 Si5 O4 109.7(3) . . ? 
O21 Si5 O4 110.4(3) . . ? 
O6 Si6 O19 111.3(4) . . ? 
O6 Si6 O18 110.1(4) . . ? 
O19 Si6 O18 108.2(4) . . ? 
O6 Si6 O5 109.1(3) . . ? 
O19 Si6 O5 109.9(4) . . ? 
O18 Si6 O5 108.2(4) . . ? 
O7 Si7 O17 109.5(4) . . ? 
O7 Si7 O48 107.5(4) . 2 ? 
O17 Si7 O48 111.5(4) . 2 ? 
O7 Si7 O23 110.0(3) . . ? 
O17 Si7 O23 108.0(3) . . ? 
O48 Si7 O23 110.4(3) 2 . ? 
O13 Si8 O12 107.5(3) . . ? 
O13 Si8 O8 110.1(3) . . ? 
O12 Si8 O8 110.6(4) . . ? 
O13 Si8 O7 110.0(4) . . ? 
O12 Si8 O7 110.2(4) . . ? 
O8 Si8 O7 108.4(4) . . ? 
O8 Si9 O25 108.4(3) . . ? 
O8 Si9 O44 111.2(4) . 4_565 ? 
O25 Si9 O44 108.4(3) . 4_565 ? 
O8 Si9 O9 108.5(4) . . ? 
O25 Si9 O9 111.0(3) . . ? 
O44 Si9 O9 109.3(3) 4_565 . ? 
O10 Si10 O26 108.7(3) . . ? 
O10 Si10 O9 109.1(4) . . ? 
O26 Si10 O9 110.7(3) . . ? 
O10 Si10 O41 110.4(4) . 4_565 ? 
O26 Si10 O41 108.1(3) . 4_565 ? 
O9 Si10 O41 109.8(3) . 4_565 ? 
O14 Si11 O10 107.7(4) . . ? 
O14 Si11 O22 110.8(3) . . ? 
O10 Si11 O22 108.6(4) . . ? 
O14 Si11 O11 110.0(4) . . ? 
O10 Si11 O11 111.1(4) . . ? 
O22 Si11 O11 108.6(4) . . ? 
O11 Si12 O24 110.5(3) . . ? 
O11 Si12 O12 108.8(4) . . ? 
O24 Si12 O12 112.4(3) . . ? 
O11 Si12 O20 109.7(4) . . ? 
O24 Si12 O20 107.3(3) . . ? 
O12 Si12 O20 108.1(3) . . ? 
O42 Si13 O21 110.0(4) . 2 ? 
O42 Si13 O27 109.6(4) . . ? 
O21 Si13 O27 109.1(3) 2 . ? 
O42 Si13 O41 110.0(4) . . ? 
O21 Si13 O41 107.5(4) 2 . ? 
O27 Si13 O41 110.6(4) . . ? 
O27 Si14 O32 109.3(4) . . ? 
O27 Si14 O39 110.6(4) . . ? 
O32 Si14 O39 108.2(4) . . ? 
O27 Si14 O28 108.1(3) . . ? 
O32 Si14 O28 109.8(3) . . ? 
O39 Si14 O28 110.8(3) . . ? 
O20 Si15 O19 109.8(3) 4_566 4_566 ? 
O20 Si15 O29 110.2(4) 4_566 . ? 
O19 Si15 O29 109.5(4) 4_566 . ? 
O20 Si15 O28 108.6(3) 4_566 . ? 
O19 Si15 O28 109.7(4) 4_566 . ? 
O29 Si15 O28 109.0(3) . . ? 
O30 Si16 O16 109.4(4) . 4_566 ? 
O30 Si16 O29 109.9(3) . . ? 
O16 Si16 O29 110.3(4) 4_566 . ? 
O30 Si16 O17 109.4(4) . 4_566 ? 
O16 Si16 O17 108.8(4) 4_566 4_566 ? 
O29 Si16 O17 109.0(4) . 4_566 ? 
O40 Si17 O47 110.6(3) . . ? 
O40 Si17 O30 108.4(4) . . ? 
O47 Si17 O30 108.2(3) . . ? 
O40 Si17 O31 109.8(4) . . ? 
O47 Si17 O31 108.9(3) . . ? 
O30 Si17 O31 110.8(4) . . ? 
O31 Si18 O44 107.3(3) . . ? 
O31 Si18 O45 110.0(4) . . ? 
O44 Si18 O45 110.5(3) . . ? 
O31 Si18 O32 109.6(3) . . ? 
O44 Si18 O32 110.3(4) . . ? 
O45 Si18 O32 109.2(3) . . ? 
O23 Si19 O22 110.8(3) . 2 ? 
O23 Si19 O33 110.1(3) . . ? 
O22 Si19 O33 108.5(4) 2 . ? 
O23 Si19 O43 107.1(3) . . ? 
O22 Si19 O43 109.5(4) 2 . ? 
O33 Si19 O43 110.9(4) . . ? 
O39 Si20 O33 109.7(4) . . ? 
O39 Si20 O34 110.4(3) . . ? 
O33 Si20 O34 108.4(3) . . ? 
O39 Si20 O38 109.8(4) . . ? 
O33 Si20 O38 109.9(4) . . ? 
O34 Si20 O38 108.6(3) . . ? 
O18 Si21 O34 108.9(3) 4_566 . ? 
O18 Si21 O35 110.0(4) 4_566 . ? 
O34 Si21 O35 108.3(3) . . ? 
O18 Si21 O25 107.6(3) 4_566 . ? 
O34 Si21 O25 111.7(3) . . ? 
O35 Si21 O25 110.3(3) . . ? 
O36 Si22 O15 110.3(4) . 4_566 ? 
O36 Si22 O35 108.1(4) . . ? 
O15 Si22 O35 109.4(3) 4_566 . ? 
O36 Si22 O26 109.8(3) . . ? 
O15 Si22 O26 108.8(3) 4_566 . ? 
O35 Si22 O26 110.4(3) . . ? 
O36 Si23 O48 109.8(4) . . ? 
O36 Si23 O37 110.4(4) . . ? 
O48 Si23 O37 107.5(4) . . ? 
O36 Si23 O40 109.7(4) . . ? 
O48 Si23 O40 110.5(3) . . ? 
O37 Si23 O40 108.9(4) . . ? 
O38 Si24 O37 109.1(4) . . ? 
O38 Si24 O24 108.4(3) . . ? 
O37 Si24 O24 109.3(3) . . ? 
O38 Si24 O46 111.3(4) . 4_666 ? 
O37 Si24 O46 111.3(4) . 4_666 ? 
O24 Si24 O46 107.5(3) . 4_666 ? 
Si2 O1 Si1 147.8(5) . . ? 
Si3 O2 Si2 148.8(4) . . ? 
Si3 O3 Si4 165.2(5) . . ? 
Si4 O4 Si5 150.7(4) . . ? 
Si6 O5 Si5 149.0(4) . . ? 
Si6 O6 Si2 162.5(5) . . ? 
Si7 O7 Si8 157.8(5) . . ? 
Si9 O8 Si8 155.0(5) . . ? 
Si10 O9 Si9 151.6(4) . . ? 
Si10 O10 Si11 158.9(5) . . ? 
Si12 O11 Si11 155.4(5) . . ? 
Si8 O12 Si12 171.8(5) . . ? 
Si8 O13 Si2 169.0(5) . . ? 
Si11 O14 Si5 162.5(4) . . ? 
Si1 O15 Si22 151.0(5) . 4_665 ? 
Si16 O16 Si1 178.2(5) 4_665 . ? 
Si7 O17 Si16 148.7(5) . 4_665 ? 
Si21 O18 Si6 143.6(4) 4_665 . ? 
Si15 O19 Si6 167.9(5) 4_665 . ? 
Si15 O20 Si12 145.9(4) 4_665 . ? 
Si13 O21 Si5 145.2(4) 2_545 . ? 
Si19 O22 Si11 152.5(5) 2_545 . ? 
Si19 O23 Si7 154.3(3) . . ? 
Si12 O24 Si24 148.3(3) . . ? 
Si9 O25 Si21 151.7(3) . . ? 
Si10 O26 Si22 146.6(3) . . ? 
Si14 O27 Si13 153.2(5) . . ? 
Si15 O28 Si14 150.6(4) . . ? 
Si15 O29 Si16 165.5(4) . . ? 
Si16 O30 Si17 160.0(5) . . ? 
Si18 O31 Si17 149.8(5) . . ? 
Si14 O32 Si18 159.3(5) . . ? 
Si20 O33 Si19 152.5(5) . . ? 
Si21 O34 Si20 149.9(4) . . ? 
Si21 O35 Si22 152.1(4) . . ? 
Si23 O36 Si22 163.1(5) . . ? 
Si24 O37 Si23 154.3(5) . . ? 
Si24 O38 Si20 156.2(5) . . ? 
Si20 O39 Si14 168.4(5) . . ? 
Si17 O40 Si23 165.3(4) . . ? 
Si10 O41 Si13 149.1(4) 4_666 . ? 
Si4 O42 Si13 162.1(5) 4_666 . ? 
Si4 O43 Si19 149.4(4) 4_666 . ? 
Si18 O44 Si9 148.3(4) . 4_666 ? 
Si3 O45 Si18 157.2(5) 4_666 . ? 
Si3 O46 Si24 153.2(5) . 4_565 ? 
Si1 O47 Si17 149.8(4) 2_545 . ? 
Si23 O48 Si7 148.2(5) . 2_545 ? 
  
_diffrn_measured_fraction_theta_max    0.935 
_diffrn_reflns_theta_full              28.65 
_diffrn_measured_fraction_theta_full   0.935 
_refine_diff_density_max    0.623 
_refine_diff_density_min   -0.572 
_refine_diff_density_rms    0.126 



  
data_f_t2butene_twin_96h 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C7.6 H0 O48 Si24' 
_chemical_formula_weight          1533
  
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' 
 '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' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    13.465(7) 
_cell_length_b                    20.177(11) 
_cell_length_c                    19.962(11) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.052(6) 
_cell_angle_gamma                 90.00 
_cell_volume                      5423(5) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.17 
_exptl_crystal_size_mid           0.13 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.835 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3008 
_exptl_absorpt_coefficient_mu     0.668 
_exptl_absorpt_correction_type    Analytical 
_exptl_absorpt_correction_T_min   0.8950 
_exptl_absorpt_correction_T_max   0.9461 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       296(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   'Bruker P4' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             62855 
_diffrn_reflns_av_R_equivalents   0.0640 
_diffrn_reflns_av_sigmaI/netI     0.0789 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        27 
_diffrn_reflns_limit_l_min        -26 
_diffrn_reflns_limit_l_max        26 
_diffrn_reflns_theta_min          1.01 
_diffrn_reflns_theta_max          28.55 
_reflns_number_total              12984 
_reflns_number_gt                 6609 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker XSCANS' 
_computing_cell_refinement        'Bruker XSCANS' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_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)+(0.0605P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none 
_refine_ls_hydrogen_treatment     none 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          12984 
_refine_ls_number_parameters      674 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1043 
_refine_ls_R_factor_gt            0.0464 
_refine_ls_wR_factor_ref          0.1404 
_refine_ls_wR_factor_gt           0.1244 
_refine_ls_goodness_of_fit_ref    0.920 
_refine_ls_restrained_S_all       0.920 
_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 
C101 C 0.9908(11) 0.4921(8) 0.4281(5) 0.104(11) Uiso 0.399(9) 1 d PG . 1 
C102 C 0.9728(13) 0.5147(9) 0.4991(5) 0.110(12) Uiso 0.399(9) 1 d PG . 1 
C103 C 1.0108(13) 0.4843(10) 0.5534(5) 0.22(3) Uiso 0.399(9) 1 d PG . 1 
C104 C 0.9929(16) 0.5068(11) 0.6243(5) 0.111(11) Uiso 0.399(9) 1 d PG . 1 
C201 C 0.9986(10) 0.4955(7) 0.0317(5) 0.089(7) Uiso 0.50 1 d PG . 2 
C202 C 0.9717(10) 0.5181(6) 0.1014(5) 0.209(17) Uiso 0.50 1 d PG . 2 
C203 C 1.0081(8) 0.4904(6) 0.1576(5) 0.182(14) Uiso 0.50 1 d PG . 2 
C204 C 0.9812(9) 0.5131(6) 0.2272(5) 0.35(3) Uiso 0.50 1 d PG . 2 
C301 C 0.6376(10) 0.2087(8) 0.2385(7) 0.234(13) Uiso 0.730(19) 1 d PG A 3 
C302 C 0.6481(8) 0.2764(8) 0.2698(6) 0.245(13) Uiso 0.730(19) 1 d PG A 3 
C303 C 0.6425(6) 0.3336(8) 0.2351(6) 0.292(17) Uiso 0.730(19) 1 d PG A 3 
C304 C 0.6529(6) 0.4013(8) 0.2664(5) 0.44(3) Uiso 0.730(19) 1 d PG A 3 
C501 C 0.5928(8) 0.2640(9) 0.2544(6) 0.31(4) Uiso 0.270(19) 1 d PG A 4 
C502 C 0.6648(6) 0.3210(7) 0.2498(6) 0.124(18) Uiso 0.270(19) 1 d PG A 4 
C503 C 0.6382(6) 0.3852(8) 0.2559(6) 0.115(17) Uiso 0.270(19) 1 d PG A 4 
C504 C 0.7102(7) 0.4422(7) 0.2513(5) 0.25(3) Uiso 0.270(19) 1 d PG A 4 
Si1 Si 0.83206(16) 0.07832(11) 0.44302(14) 0.0166(5) Uani 1 1 d . . . 
Si2 Si 0.68280(18) 0.19084(12) 0.47002(10) 0.0192(5) Uani 1 1 d . . . 
Si3 Si 0.46258(16) 0.22017(11) 0.43811(13) 0.0194(5) Uani 1 1 d . . . 
Si4 Si 0.47067(16) 0.37706(11) 0.43635(12) 0.0160(5) Uani 1 1 d . . . 
Si5 Si 0.68235(18) 0.42640(11) 0.47162(11) 0.0158(5) Uani 1 1 d . . . 
Si6 Si 0.82537(16) 0.31113(11) 0.44183(13) 0.0190(5) Uani 1 1 d . . . 
Si7 Si 0.82500(18) 0.07658(11) 0.67180(12) 0.0170(5) Uani 1 1 d . . . 
Si8 Si 0.68400(17) 0.19194(12) 0.62803(12) 0.0173(5) Uani 1 1 d . . . 
Si9 Si 0.46998(16) 0.22663(11) 0.67415(12) 0.0167(5) Uani 1 1 d . . . 
Si10 Si 0.47245(17) 0.38053(12) 0.67443(12) 0.0181(5) Uani 1 1 d . . . 
Si11 Si 0.68322(18) 0.42963(10) 0.62933(12) 0.0165(5) Uani 1 1 d . . . 
Si12 Si 0.82098(17) 0.31307(11) 0.66995(11) 0.0168(5) Uani 1 1 d . . . 
Si13 Si 0.83844(16) 0.07497(10) 1.05743(14) 0.0160(5) Uani 1 1 d . . . 
Si14 Si 0.69287(17) 0.19083(13) 1.02854(10) 0.0185(5) Uani 1 1 d . . . 
Si15 Si 0.47248(15) 0.22052(11) 1.06133(13) 0.0167(5) Uani 1 1 d . . . 
Si16 Si 0.47218(16) 0.37734(11) 1.06354(12) 0.0166(5) Uani 1 1 d . . . 
Si17 Si 0.68599(17) 0.42904(11) 1.02846(11) 0.0138(5) Uani 1 1 d . . . 
Si18 Si 0.82711(16) 0.31461(11) 1.06120(13) 0.0177(5) Uani 1 1 d . . . 
Si19 Si 0.82247(18) 0.07693(11) 0.82774(12) 0.0160(5) Uani 1 1 d . . . 
Si20 Si 0.68230(18) 0.19137(12) 0.86995(12) 0.0182(5) Uani 1 1 d . . . 
Si21 Si 0.46600(17) 0.22626(11) 0.82982(12) 0.0176(5) Uani 1 1 d . . . 
Si22 Si 0.47008(17) 0.38136(12) 0.82819(12) 0.0175(5) Uani 1 1 d . . . 
Si23 Si 0.68296(19) 0.42974(10) 0.87006(12) 0.0166(5) Uani 1 1 d . . . 
Si24 Si 0.81357(17) 0.31166(11) 0.82409(11) 0.0180(5) Uani 1 1 d . . . 
O1 O 0.7385(4) 0.1269(3) 0.4442(4) 0.0427(17) Uani 1 1 d . . . 
O2 O 0.5742(4) 0.1920(3) 0.4379(3) 0.0347(15) Uani 1 1 d . . . 
O3 O 0.4628(5) 0.2984(3) 0.4446(4) 0.0486(17) Uani 1 1 d . . . 
O4 O 0.5849(4) 0.3990(3) 0.4363(3) 0.0350(15) Uani 1 1 d . . . 
O5 O 0.7781(4) 0.3836(3) 0.4480(3) 0.0307(14) Uani 1 1 d . . . 
O6 O 0.7410(5) 0.2566(3) 0.4498(4) 0.0523(19) Uani 1 1 d . . . 
O7 O 0.7391(5) 0.1281(3) 0.6573(4) 0.045(2) Uani 1 1 d . . . 
O8 O 0.5754(4) 0.1960(3) 0.6609(3) 0.0427(17) Uani 1 1 d . . . 
O9 O 0.4728(5) 0.3035(3) 0.6544(3) 0.0336(16) Uani 1 1 d . . . 
O10 O 0.5806(4) 0.4105(3) 0.6656(3) 0.0382(16) Uani 1 1 d . . . 
O11 O 0.7724(4) 0.3832(3) 0.6546(3) 0.0333(16) Uani 1 1 d . . . 
O12 O 0.7465(5) 0.2563(3) 0.6477(3) 0.0435(18) Uani 1 1 d . . . 
O13 O 0.6760(5) 0.1869(4) 0.5495(3) 0.063(2) Uani 1 1 d . . . 
O14 O 0.6679(4) 0.4214(3) 0.5516(3) 0.0373(15) Uani 1 1 d . . . 
O15 O 0.8884(5) 0.0829(3) 0.3730(3) 0.0386(17) Uani 1 1 d . . . 
O16 O 0.9065(5) 0.0965(4) 0.5019(3) 0.0482(19) Uani 1 1 d . . . 
O17 O 0.9223(4) 0.0999(3) 0.6340(3) 0.0301(15) Uani 1 1 d . . . 
O18 O 0.8748(4) 0.3057(3) 0.3707(3) 0.0334(15) Uani 1 1 d . . . 
O19 O 0.9104(5) 0.3013(3) 0.4975(3) 0.0415(16) Uani 1 1 d . . . 
O20 O 0.9225(4) 0.3056(3) 0.6290(3) 0.0330(15) Uani 1 1 d . . . 
O21 O 0.7042(4) 0.5015(2) 0.4484(3) 0.0285(14) Uani 1 1 d . . . 
O22 O 0.7108(4) 0.5040(3) 0.6481(3) 0.0306(15) Uani 1 1 d . . . 
O23 O 0.8493(2) 0.07595(17) 0.7502(4) 0.0357(9) Uani 1 1 d . . . 
O24 O 0.8469(2) 0.30657(16) 0.7484(3) 0.0314(8) Uani 1 1 d . . . 
O25 O 0.4438(2) 0.21706(15) 0.7500(3) 0.0279(8) Uani 1 1 d . . . 
O26 O 0.4387(2) 0.39005(15) 0.7508(3) 0.0257(8) Uani 1 1 d . . . 
O27 O 0.7482(4) 0.1269(3) 1.0573(4) 0.0406(17) Uani 1 1 d . . . 
O28 O 0.5807(4) 0.1902(3) 1.0562(3) 0.0317(14) Uani 1 1 d . . . 
O29 O 0.4798(5) 0.2997(3) 1.0621(4) 0.0511(18) Uani 1 1 d . . . 
O30 O 0.5795(4) 0.4086(3) 1.0603(3) 0.0381(15) Uani 1 1 d . . . 
O31 O 0.7703(4) 0.3838(3) 1.0592(3) 0.0316(14) Uani 1 1 d . . . 
O32 O 0.7472(4) 0.2551(3) 1.0568(3) 0.0367(15) Uani 1 1 d . . . 
O33 O 0.7307(4) 0.1260(3) 0.8407(3) 0.0340(17) Uani 1 1 d . . . 
O34 O 0.5667(4) 0.1904(3) 0.8509(3) 0.0339(15) Uani 1 1 d . . . 
O35 O 0.4741(5) 0.3043(3) 0.8478(3) 0.0348(17) Uani 1 1 d . . . 
O36 O 0.5779(5) 0.4120(3) 0.8406(3) 0.055(2) Uani 1 1 d . . . 
O37 O 0.7647(5) 0.3824(3) 0.8375(3) 0.0414(18) Uani 1 1 d . . . 
O38 O 0.7319(5) 0.2563(3) 0.8378(3) 0.0516(19) Uani 1 1 d . . . 
O39 O 0.6944(5) 0.1918(4) 0.9490(3) 0.0601(19) Uani 1 1 d . . . 
O40 O 0.6818(5) 0.4188(3) 0.9500(3) 0.0369(15) Uani 1 1 d . . . 
O41 O 0.8959(5) 0.0799(3) 1.1276(3) 0.0360(17) Uani 1 1 d . . . 
O42 O 0.9151(5) 0.0896(3) 0.9979(3) 0.0371(16) Uani 1 1 d . . . 
O43 O 0.9209(4) 0.1005(3) 0.8689(3) 0.0350(16) Uani 1 1 d . . . 
O44 O 0.8877(4) 0.3096(3) 1.1306(3) 0.0295(14) Uani 1 1 d . . . 
O45 O 0.9025(5) 0.3115(3) 0.9986(3) 0.0366(15) Uani 1 1 d . . . 
O46 O 0.4115(4) 0.1992(3) 0.3697(3) 0.0450(18) Uani 1 1 d . . . 
O47 O 0.7088(4) 0.5042(2) 1.0457(3) 0.0246(14) Uani 1 1 d . . . 
O48 O 0.7096(4) 0.5057(3) 0.8539(3) 0.0332(16) Uani 1 1 d . . . 
  
  
_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 
C101 C103 0.60(3) 3_766 ? 
C101 C104 1.07(2) 3_766 ? 
C101 C102 1.5079 . ? 
C101 C102 1.54(2) 3_766 ? 
C102 C102 0.94(4) 3_766 ? 
C102 C103 1.07(2) 3_766 ? 
C102 C103 1.3461 . ? 
C102 C101 1.54(2) 3_766 ? 
C103 C101 0.60(3) 3_766 ? 
C103 C102 1.07(2) 3_766 ? 
C103 C104 1.5079 . ? 
C104 C101 1.07(2) 3_766 ? 
C201 C201 1.28(2) 3_765 ? 
C201 C202 1.5083 . ? 
C202 C203 1.3464 . ? 
C203 C204 1.5063 . ? 
C301 C302 1.5092 . ? 
C302 C303 1.3473 . ? 
C303 C304 1.5090 . ? 
C501 C502 1.5078 . ? 
C502 C503 1.3484 . ? 
C503 C504 1.5076 . ? 
Si1 O16 1.586(6) . ? 
Si1 O15 1.593(6) . ? 
Si1 O1 1.596(6) . ? 
Si1 O47 1.608(5) 2_646 ? 
Si2 O1 1.579(6) . ? 
Si2 O13 1.591(7) . ? 
Si2 O6 1.593(6) . ? 
Si2 O2 1.596(6) . ? 
Si3 O3 1.584(6) . ? 
Si3 O46 1.587(6) . ? 
Si3 O45 1.588(6) 4_565 ? 
Si3 O2 1.607(6) . ? 
Si4 O43 1.571(6) 4_565 ? 
Si4 O42 1.588(6) 4_565 ? 
Si4 O3 1.599(6) . ? 
Si4 O4 1.600(6) . ? 
Si5 O4 1.589(6) . ? 
Si5 O14 1.611(7) . ? 
Si5 O21 1.612(6) . ? 
Si5 O5 1.623(6) . ? 
Si6 O18 1.573(6) . ? 
Si6 O6 1.590(6) . ? 
Si6 O5 1.599(5) . ? 
Si6 O19 1.607(6) . ? 
Si7 O7 1.582(6) . ? 
Si7 O17 1.584(6) . ? 
Si7 O48 1.590(6) 2_646 ? 
Si7 O23 1.599(7) . ? 
Si8 O13 1.575(7) . ? 
Si8 O12 1.596(6) . ? 
Si8 O7 1.597(6) . ? 
Si8 O8 1.606(6) . ? 
Si9 O25 1.568(7) . ? 
Si9 O8 1.570(6) . ? 
Si9 O44 1.586(6) 4_565 ? 
Si9 O9 1.601(6) . ? 
Si10 O10 1.587(6) . ? 
Si10 O26 1.602(7) . ? 
Si10 O41 1.604(6) 4_565 ? 
Si10 O9 1.605(6) . ? 
Si11 O14 1.575(7) . ? 
Si11 O22 1.591(6) . ? 
Si11 O11 1.604(6) . ? 
Si11 O10 1.608(6) . ? 
Si12 O12 1.586(6) . ? 
Si12 O11 1.589(6) . ? 
Si12 O20 1.599(6) . ? 
Si12 O24 1.609(7) . ? 
Si13 O21 1.593(5) 2_646 ? 
Si13 O41 1.602(6) . ? 
Si13 O42 1.602(6) . ? 
Si13 O27 1.605(6) . ? 
Si14 O39 1.588(6) . ? 
Si14 O32 1.592(6) . ? 
Si14 O27 1.596(6) . ? 
Si14 O28 1.608(6) . ? 
Si15 O28 1.584(6) . ? 
Si15 O19 1.585(6) 4_566 ? 
Si15 O20 1.600(6) 4_566 ? 
Si15 O29 1.601(6) . ? 
Si16 O29 1.570(6) . ? 
Si16 O30 1.578(6) . ? 
Si16 O16 1.605(6) 4_566 ? 
Si16 O17 1.626(6) 4_566 ? 
Si17 O31 1.580(6) . ? 
Si17 O40 1.581(6) . ? 
Si17 O47 1.586(5) . ? 
Si17 O30 1.623(6) . ? 
Si18 O31 1.593(6) . ? 
Si18 O44 1.610(6) . ? 
Si18 O45 1.612(6) . ? 
Si18 O32 1.614(6) . ? 
Si19 O23 1.589(7) . ? 
Si19 O33 1.605(6) . ? 
Si19 O22 1.612(6) 2_646 ? 
Si19 O43 1.630(6) . ? 
Si20 O33 1.583(6) . ? 
Si20 O39 1.586(6) . ? 
Si20 O34 1.603(6) . ? 
Si20 O38 1.604(6) . ? 
Si21 O34 1.592(6) . ? 
Si21 O18 1.610(6) 4_566 ? 
Si21 O35 1.619(6) . ? 
Si21 O25 1.631(7) . ? 
Si22 O15 1.591(6) 4_566 ? 
Si22 O36 1.597(7) . ? 
Si22 O35 1.604(6) . ? 
Si22 O26 1.612(7) . ? 
Si23 O36 1.572(7) . ? 
Si23 O37 1.596(6) . ? 
Si23 O48 1.606(6) . ? 
Si23 O40 1.611(6) . ? 
Si24 O24 1.580(7) . ? 
Si24 O38 1.592(6) . ? 
Si24 O37 1.594(7) . ? 
Si24 O46 1.616(6) 4_666 ? 
O15 Si22 1.591(6) 4_665 ? 
O16 Si16 1.605(6) 4_665 ? 
O17 Si16 1.626(6) 4_665 ? 
O18 Si21 1.610(6) 4_665 ? 
O19 Si15 1.585(6) 4_665 ? 
O20 Si15 1.600(6) 4_665 ? 
O21 Si13 1.593(5) 2_656 ? 
O22 Si19 1.612(6) 2_656 ? 
O41 Si10 1.604(6) 4_666 ? 
O42 Si4 1.588(6) 4_666 ? 
O43 Si4 1.571(6) 4_666 ? 
O44 Si9 1.586(6) 4_666 ? 
O45 Si3 1.588(6) 4_666 ? 
O46 Si24 1.616(6) 4_565 ? 
O47 Si1 1.609(5) 2_656 ? 
O48 Si7 1.590(6) 2_656 ? 
  
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 
C103 C101 C104 126(4) 3_766 3_766 ? 
C103 C101 C102 35(3) 3_766 . ? 
C104 C101 C102 161.2(15) 3_766 . ? 
C103 C101 C102 60.3(19) 3_766 3_766 ? 
C104 C101 C102 149(3) 3_766 3_766 ? 
C102 C101 C102 36.0(14) . 3_766 ? 
C102 C102 C103 84(2) 3_766 3_766 ? 
C102 C102 C103 52.2(14) 3_766 . ? 
C103 C102 C103 135.9(19) 3_766 . ? 
C102 C102 C101 73.8(13) 3_766 . ? 
C103 C102 C101 18.8(17) 3_766 . ? 
C103 C102 C101 123.8 . . ? 
C102 C102 C101 70.2(15) 3_766 3_766 ? 
C103 C102 C101 149(3) 3_766 3_766 ? 
C103 C102 C101 22.9(14) . 3_766 ? 
C101 C102 C101 144.0(14) . 3_766 ? 
C101 C103 C102 126(5) 3_766 3_766 ? 
C101 C103 C102 97(3) 3_766 . ? 
C102 C103 C102 44(2) 3_766 . ? 
C101 C103 C104 35(3) 3_766 . ? 
C102 C103 C104 161.2(19) 3_766 . ? 
C102 C103 C104 123.8 . . ? 
C101 C104 C103 18.8(19) 3_766 . ? 
C201 C201 C202 151.3(16) 3_765 . ? 
C203 C202 C201 123.8 . . ? 
C202 C203 C204 123.8 . . ? 
C303 C302 C301 123.9 . . ? 
C302 C303 C304 123.9 . . ? 
C503 C502 C501 123.8 . . ? 
C502 C503 C504 123.7 . . ? 
O16 Si1 O15 109.6(3) . . ? 
O16 Si1 O1 110.2(4) . . ? 
O15 Si1 O1 110.7(4) . . ? 
O16 Si1 O47 109.0(3) . 2_646 ? 
O15 Si1 O47 109.9(3) . 2_646 ? 
O1 Si1 O47 107.4(3) . 2_646 ? 
O1 Si2 O13 108.2(4) . . ? 
O1 Si2 O6 111.3(4) . . ? 
O13 Si2 O6 108.8(4) . . ? 
O1 Si2 O2 108.4(3) . . ? 
O13 Si2 O2 110.3(4) . . ? 
O6 Si2 O2 109.7(3) . . ? 
O3 Si3 O46 109.7(4) . . ? 
O3 Si3 O45 109.9(4) . 4_565 ? 
O46 Si3 O45 109.1(4) . 4_565 ? 
O3 Si3 O2 110.6(3) . . ? 
O46 Si3 O2 108.0(4) . . ? 
O45 Si3 O2 109.6(4) 4_565 . ? 
O43 Si4 O42 109.9(3) 4_565 4_565 ? 
O43 Si4 O3 110.3(4) 4_565 . ? 
O42 Si4 O3 108.0(4) 4_565 . ? 
O43 Si4 O4 109.2(4) 4_565 . ? 
O42 Si4 O4 109.7(4) 4_565 . ? 
O3 Si4 O4 109.8(3) . . ? 
O4 Si5 O14 108.5(3) . . ? 
O4 Si5 O21 110.5(3) . . ? 
O14 Si5 O21 111.5(3) . . ? 
O4 Si5 O5 110.0(3) . . ? 
O14 Si5 O5 110.6(3) . . ? 
O21 Si5 O5 105.8(3) . . ? 
O18 Si6 O6 110.2(4) . . ? 
O18 Si6 O5 107.5(4) . . ? 
O6 Si6 O5 109.9(3) . . ? 
O18 Si6 O19 108.3(4) . . ? 
O6 Si6 O19 110.7(4) . . ? 
O5 Si6 O19 110.1(4) . . ? 
O7 Si7 O17 108.8(4) . . ? 
O7 Si7 O48 108.6(4) . 2_646 ? 
O17 Si7 O48 110.9(3) . 2_646 ? 
O7 Si7 O23 109.5(3) . . ? 
O17 Si7 O23 107.4(3) . . ? 
O48 Si7 O23 111.6(3) 2_646 . ? 
O13 Si8 O12 109.5(4) . . ? 
O13 Si8 O7 110.0(4) . . ? 
O12 Si8 O7 108.7(4) . . ? 
O13 Si8 O8 110.4(4) . . ? 
O12 Si8 O8 109.8(3) . . ? 
O7 Si8 O8 108.4(4) . . ? 
O25 Si9 O8 108.6(3) . . ? 
O25 Si9 O44 108.4(3) . 4_565 ? 
O8 Si9 O44 110.9(3) . 4_565 ? 
O25 Si9 O9 111.3(3) . . ? 
O8 Si9 O9 108.5(3) . . ? 
O44 Si9 O9 109.2(3) 4_565 . ? 
O10 Si10 O26 108.7(3) . . ? 
O10 Si10 O41 109.6(4) . 4_565 ? 
O26 Si10 O41 108.2(3) . 4_565 ? 
O10 Si10 O9 109.8(4) . . ? 
O26 Si10 O9 110.7(3) . . ? 
O41 Si10 O9 109.8(3) 4_565 . ? 
O14 Si11 O22 111.3(3) . . ? 
O14 Si11 O11 110.2(4) . . ? 
O22 Si11 O11 107.6(4) . . ? 
O14 Si11 O10 107.9(3) . . ? 
O22 Si11 O10 108.7(3) . . ? 
O11 Si11 O10 111.2(3) . . ? 
O12 Si12 O11 109.2(4) . . ? 
O12 Si12 O20 109.2(3) . . ? 
O11 Si12 O20 109.7(3) . . ? 
O12 Si12 O24 110.5(3) . . ? 
O11 Si12 O24 110.4(3) . . ? 
O20 Si12 O24 107.8(3) . . ? 
O21 Si13 O41 107.2(3) 2_646 . ? 
O21 Si13 O42 110.4(4) 2_646 . ? 
O41 Si13 O42 109.1(4) . . ? 
O21 Si13 O27 109.5(3) 2_646 . ? 
O41 Si13 O27 109.0(4) . . ? 
O42 Si13 O27 111.5(4) . . ? 
O39 Si14 O32 109.8(4) . . ? 
O39 Si14 O27 111.3(4) . . ? 
O32 Si14 O27 108.5(4) . . ? 
O39 Si14 O28 110.9(3) . . ? 
O32 Si14 O28 108.4(3) . . ? 
O27 Si14 O28 107.9(3) . . ? 
O28 Si15 O19 109.0(4) . 4_566 ? 
O28 Si15 O20 108.4(3) . 4_566 ? 
O19 Si15 O20 111.4(3) 4_566 4_566 ? 
O28 Si15 O29 109.3(3) . . ? 
O19 Si15 O29 108.5(4) 4_566 . ? 
O20 Si15 O29 110.3(4) 4_566 . ? 
O29 Si16 O30 109.8(3) . . ? 
O29 Si16 O16 110.5(4) . 4_566 ? 
O30 Si16 O16 110.0(4) . 4_566 ? 
O29 Si16 O17 109.0(4) . 4_566 ? 
O30 Si16 O17 107.5(4) . 4_566 ? 
O16 Si16 O17 110.1(3) 4_566 4_566 ? 
O31 Si17 O40 109.5(3) . . ? 
O31 Si17 O47 109.3(3) . . ? 
O40 Si17 O47 110.3(3) . . ? 
O31 Si17 O30 109.6(3) . . ? 
O40 Si17 O30 108.9(3) . . ? 
O47 Si17 O30 109.2(3) . . ? 
O31 Si18 O44 108.6(3) . . ? 
O31 Si18 O45 108.5(4) . . ? 
O44 Si18 O45 110.2(3) . . ? 
O31 Si18 O32 109.3(3) . . ? 
O44 Si18 O32 109.8(4) . . ? 
O45 Si18 O32 110.5(3) . . ? 
O23 Si19 O33 109.9(3) . . ? 
O23 Si19 O22 110.1(3) . 2_646 ? 
O33 Si19 O22 107.5(3) . 2_646 ? 
O23 Si19 O43 108.0(3) . . ? 
O33 Si19 O43 111.4(3) . . ? 
O22 Si19 O43 110.0(4) 2_646 . ? 
O33 Si20 O39 109.2(4) . . ? 
O33 Si20 O34 107.7(3) . . ? 
O39 Si20 O34 109.6(3) . . ? 
O33 Si20 O38 111.2(4) . . ? 
O39 Si20 O38 110.6(4) . . ? 
O34 Si20 O38 108.6(3) . . ? 
O34 Si21 O18 109.5(3) . 4_566 ? 
O34 Si21 O35 109.0(3) . . ? 
O18 Si21 O35 109.2(4) 4_566 . ? 
O34 Si21 O25 111.2(3) . . ? 
O18 Si21 O25 108.0(3) 4_566 . ? 
O35 Si21 O25 109.9(3) . . ? 
O15 Si22 O36 111.5(4) 4_566 . ? 
O15 Si22 O35 108.9(3) 4_566 . ? 
O36 Si22 O35 107.8(4) . . ? 
O15 Si22 O26 108.0(3) 4_566 . ? 
O36 Si22 O26 110.1(3) . . ? 
O35 Si22 O26 110.4(3) . . ? 
O36 Si23 O37 109.4(4) . . ? 
O36 Si23 O48 110.1(4) . . ? 
O37 Si23 O48 109.6(3) . . ? 
O36 Si23 O40 109.2(4) . . ? 
O37 Si23 O40 109.2(3) . . ? 
O48 Si23 O40 109.4(3) . . ? 
O24 Si24 O38 108.4(3) . . ? 
O24 Si24 O37 109.7(3) . . ? 
O38 Si24 O37 108.3(4) . . ? 
O24 Si24 O46 107.3(3) . 4_666 ? 
O38 Si24 O46 111.8(4) . 4_666 ? 
O37 Si24 O46 111.3(4) . 4_666 ? 
Si2 O1 Si1 151.8(5) . . ? 
Si2 O2 Si3 149.4(4) . . ? 
Si3 O3 Si4 168.7(5) . . ? 
Si5 O4 Si4 152.7(5) . . ? 
Si6 O5 Si5 145.6(4) . . ? 
Si6 O6 Si2 162.5(5) . . ? 
Si7 O7 Si8 159.5(5) . . ? 
Si9 O8 Si8 155.9(4) . . ? 
Si9 O9 Si10 151.3(4) . . ? 
Si10 O10 Si11 158.5(4) . . ? 
Si12 O11 Si11 152.8(5) . . ? 
Si12 O12 Si8 171.8(5) . . ? 
Si8 O13 Si2 170.2(5) . . ? 
Si11 O14 Si5 162.6(4) . . ? 
Si22 O15 Si1 148.2(4) 4_665 . ? 
Si1 O16 Si16 172.5(5) . 4_665 ? 
Si7 O17 Si16 146.9(4) . 4_665 ? 
Si6 O18 Si21 144.0(4) . 4_665 ? 
Si15 O19 Si6 164.7(5) 4_665 . ? 
Si12 O20 Si15 145.4(4) . 4_665 ? 
Si13 O21 Si5 146.1(4) 2_656 . ? 
Si11 O22 Si19 150.1(4) . 2_656 ? 
Si19 O23 Si7 155.1(2) . . ? 
Si24 O24 Si12 149.8(2) . . ? 
Si9 O25 Si21 152.7(2) . . ? 
Si10 O26 Si22 145.6(2) . . ? 
Si14 O27 Si13 151.8(5) . . ? 
Si15 O28 Si14 152.1(4) . . ? 
Si16 O29 Si15 172.7(5) . . ? 
Si16 O30 Si17 158.0(5) . . ? 
Si17 O31 Si18 149.4(4) . . ? 
Si14 O32 Si18 158.6(4) . . ? 
Si20 O33 Si19 153.0(5) . . ? 
Si21 O34 Si20 152.1(4) . . ? 
Si22 O35 Si21 152.4(4) . . ? 
Si23 O36 Si22 164.5(5) . . ? 
Si24 O37 Si23 152.8(5) . . ? 
Si24 O38 Si20 158.4(5) . . ? 
Si20 O39 Si14 173.3(5) . . ? 
Si17 O40 Si23 164.4(4) . . ? 
Si13 O41 Si10 148.2(4) . 4_666 ? 
Si4 O42 Si13 162.9(5) 4_666 . ? 
Si4 O43 Si19 149.6(4) 4_666 . ? 
Si9 O44 Si18 148.6(4) 4_666 . ? 
Si3 O45 Si18 157.8(5) 4_666 . ? 
Si3 O46 Si24 150.9(4) . 4_565 ? 
Si17 O47 Si1 148.6(4) . 2_656 ? 
Si7 O48 Si23 149.1(4) 2_656 . ? 
  
_diffrn_measured_fraction_theta_max    0.939 
_diffrn_reflns_theta_full              28.55 
_diffrn_measured_fraction_theta_full   0.939 
_refine_diff_density_max    0.920 
_refine_diff_density_min   -0.443 
_refine_diff_density_rms    0.111 


