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

  
data_f_seino_1-butene_twin_01_ss159 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C4.4 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                    13.455(3) 
_cell_length_b                    20.190(4) 
_cell_length_c                    19.950(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.16(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      5419.5(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           0.10 
_exptl_crystal_size_min           0.05 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.836 
_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   0.9030 
_exptl_absorpt_correction_T_max   0.9642 
_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             63783 
_diffrn_reflns_av_R_equivalents   0.1704 
_diffrn_reflns_av_sigmaI/netI     0.2384 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        -27 
_diffrn_reflns_limit_k_max        27 
_diffrn_reflns_limit_l_min        -26 
_diffrn_reflns_limit_l_max        26 
_diffrn_reflns_theta_min          1.51 
_diffrn_reflns_theta_max          28.71 
_reflns_number_total              13278 
_reflns_number_gt                 4054 
_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)+(0.0315P)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          13278 
_refine_ls_number_parameters      684 
_refine_ls_number_restraints      10 
_refine_ls_R_factor_all           0.1963 
_refine_ls_R_factor_gt            0.0525 
_refine_ls_wR_factor_ref          0.1281 
_refine_ls_wR_factor_gt           0.0983 
_refine_ls_goodness_of_fit_ref    0.738 
_refine_ls_restrained_S_all       0.741 
_refine_ls_shift/su_max           0.004 
_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 
C301 C 0.154(4) 0.260(2) 0.750(4) 0.36(3) Uiso 0.599(18) 1 d PD A 1 
C302 C 0.114(3) 0.199(3) 0.737(3) 0.34(3) Uiso 0.599(18) 1 d PD A 1 
C303 C 0.143(4) 0.136(3) 0.768(3) 0.35(3) Uiso 0.599(18) 1 d PD A 1 
C304 C 0.192(4) 0.073(3) 0.742(5) 0.51(5) Uiso 0.599(18) 1 d PD A 1 
C101 C -0.005(2) 0.5096(16) 0.5401(14) 0.120(12) Uiso 0.50 1 d PD . 2 
C102 C -0.009(3) 0.4995(17) 0.6061(15) 0.141(14) Uiso 0.50 1 d PD B 2 
C103 C 0.037(4) 0.494(3) 0.6730(18) 0.34(3) Uiso 0.50 1 d PD B 2 
C104 C 0.011(4) 0.495(3) 0.745(2) 0.37(3) Uiso 0.50 1 d PD B 2 
Si1 Si 0.3250(2) 0.42104(14) -0.05619(18) 0.0157(7) Uani 1 1 d . . . 
Si2 Si 0.1716(3) 0.31161(17) -0.03042(14) 0.0199(8) Uani 1 1 d . . . 
Si3 Si -0.0462(2) 0.27912(15) -0.06201(18) 0.0199(8) Uani 1 1 d . . . 
Si4 Si -0.0341(2) 0.12324(16) -0.06293(18) 0.0186(8) Uani 1 1 d . . . 
Si5 Si 0.1783(3) 0.07556(15) -0.02830(15) 0.0174(8) Uani 1 1 d . . . 
Si6 Si 0.3189(2) 0.19272(16) -0.05615(17) 0.0187(7) Uani 1 1 d . . . 
Si7 Si 0.3216(3) 0.42468(16) 0.17141(16) 0.0180(8) Uani 1 1 d . . . 
Si8 Si 0.1784(2) 0.31032(17) 0.12730(15) 0.0180(7) Uani 1 1 d . . . 
Si9 Si -0.0336(2) 0.27339(16) 0.17535(16) 0.0168(8) Uani 1 1 d . . . 
Si10 Si -0.0309(3) 0.11913(17) 0.17533(16) 0.0186(8) Uani 1 1 d . . . 
Si11 Si 0.1779(3) 0.07141(15) 0.12921(17) 0.0172(8) Uani 1 1 d . . . 
Si12 Si 0.3168(3) 0.18971(17) 0.16751(15) 0.0182(7) Uani 1 1 d . . . 
Si13 Si 0.3363(2) 0.42671(14) 0.55750(19) 0.0177(7) Uani 1 1 d . . . 
Si14 Si 0.1897(2) 0.31135(17) 0.52774(14) 0.0173(7) Uani 1 1 d . . . 
Si15 Si -0.0286(2) 0.27806(15) 0.56163(16) 0.0159(7) Uani 1 1 d . . . 
Si16 Si -0.0313(2) 0.12204(16) 0.56369(18) 0.0179(8) Uani 1 1 d . . . 
Si17 Si 0.1815(3) 0.07058(15) 0.52782(15) 0.0148(7) Uani 1 1 d . . . 
Si18 Si 0.3209(2) 0.18668(15) 0.56202(16) 0.0180(7) Uani 1 1 d . . . 
Si19 Si 0.3179(3) 0.42349(15) 0.32775(16) 0.0169(8) Uani 1 1 d . . . 
Si20 Si 0.1737(2) 0.31114(17) 0.36914(16) 0.0181(7) Uani 1 1 d . . . 
Si21 Si -0.0408(3) 0.27365(16) 0.33095(16) 0.0194(8) Uani 1 1 d . . . 
Si22 Si -0.0353(3) 0.11879(17) 0.32899(16) 0.0183(8) Uani 1 1 d . . . 
Si23 Si 0.1792(3) 0.07174(14) 0.36961(17) 0.0172(7) Uani 1 1 d . . . 
Si24 Si 0.3046(2) 0.19164(17) 0.32198(14) 0.0183(7) Uani 1 1 d . . . 
O1 O 0.2270(5) 0.3755(4) -0.0582(5) 0.034(2) Uani 1 1 d . . . 
O2 O 0.0630(5) 0.3093(4) -0.0638(4) 0.0267(18) Uani 1 1 d . . . 
O3 O -0.0451(6) 0.2011(3) -0.0521(4) 0.043(2) Uani 1 1 d . . . 
O4 O 0.0789(5) 0.1020(4) -0.0658(4) 0.030(2) Uani 1 1 d . . . 
O5 O 0.2720(5) 0.1203(3) -0.0474(4) 0.026(2) Uani 1 1 d . . . 
O6 O 0.2327(6) 0.2459(4) -0.0469(5) 0.040(2) Uani 1 1 d . . . 
O7 O 0.2309(7) 0.3743(4) 0.1556(4) 0.041(3) Uani 1 1 d . . . 
O8 O 0.0734(5) 0.3038(4) 0.1646(3) 0.036(2) Uani 1 1 d . . . 
O9 O -0.0301(6) 0.1960(4) 0.1555(3) 0.031(2) Uani 1 1 d . . . 
O10 O 0.0776(6) 0.0895(4) 0.1667(4) 0.037(2) Uani 1 1 d . . . 
O11 O 0.2653(7) 0.1206(4) 0.1515(4) 0.035(2) Uani 1 1 d . . . 
O12 O 0.2437(6) 0.2472(4) 0.1417(4) 0.041(2) Uani 1 1 d . . . 
O13 O 0.1616(6) 0.3167(4) 0.0484(4) 0.047(2) Uani 1 1 d . . . 
O14 O 0.1586(5) 0.0785(3) 0.0505(4) 0.032(2) Uani 1 1 d . . . 
O15 O 0.3806(6) 0.4137(4) -0.1259(4) 0.031(2) Uani 1 1 d . . . 
O16 O 0.3962(7) 0.3976(4) 0.0033(4) 0.045(3) Uani 1 1 d . . . 
O17 O 0.4178(6) 0.4014(4) 0.1331(4) 0.031(2) Uani 1 1 d . . . 
O18 O 0.3664(5) 0.1973(4) -0.1286(4) 0.031(2) Uani 1 1 d . . . 
O19 O 0.4039(6) 0.2042(4) -0.0019(4) 0.039(2) Uani 1 1 d . . . 
O20 O 0.4207(5) 0.1962(4) 0.1284(4) 0.0270(18) Uani 1 1 d . . . 
O21 O 0.2027(5) 0.0015(3) -0.0515(4) 0.0251(19) Uani 1 1 d . . . 
O22 O 0.2088(6) -0.0039(4) 0.1475(4) 0.031(2) Uani 1 1 d . . . 
O23 O 0.3450(4) 0.4240(3) 0.2501(5) 0.0335(15) Uani 1 1 d . . . 
O24 O 0.3408(4) 0.1972(3) 0.2457(4) 0.0306(14) Uani 1 1 d . . . 
O25 O -0.0627(4) 0.2826(2) 0.2531(4) 0.0290(15) Uani 1 1 d . . . 
O26 O -0.0660(4) 0.1099(2) 0.2518(5) 0.0258(15) Uani 1 1 d . . . 
O27 O 0.2467(5) 0.3764(4) 0.5525(5) 0.038(2) Uani 1 1 d . . . 
O28 O 0.0777(5) 0.3132(3) 0.5548(4) 0.0304(19) Uani 1 1 d . . . 
O29 O -0.0138(5) 0.2007(3) 0.5652(4) 0.040(2) Uani 1 1 d . . . 
O30 O 0.0727(6) 0.0857(4) 0.5563(5) 0.040(2) Uani 1 1 d . . . 
O31 O 0.2610(6) 0.1190(4) 0.5641(4) 0.031(2) Uani 1 1 d . . . 
O32 O 0.2448(6) 0.2485(4) 0.5588(4) 0.034(2) Uani 1 1 d . . . 
O33 O 0.2236(6) 0.3777(4) 0.3415(4) 0.031(2) Uani 1 1 d . . . 
O34 O 0.0575(5) 0.3128(3) 0.3534(3) 0.0249(18) Uani 1 1 d . . . 
O35 O -0.0250(6) 0.1966(4) 0.3479(3) 0.034(2) Uani 1 1 d . . . 
O36 O 0.0703(6) 0.0831(4) 0.3433(4) 0.040(2) Uani 1 1 d . . . 
O37 O 0.2574(7) 0.1208(4) 0.3339(4) 0.036(2) Uani 1 1 d . . . 
O38 O 0.2222(6) 0.2477(4) 0.3342(4) 0.035(2) Uani 1 1 d . . . 
O39 O 0.1922(6) 0.3062(5) 0.4489(4) 0.053(2) Uani 1 1 d . . . 
O40 O 0.1840(6) 0.0829(4) 0.4487(4) 0.037(2) Uani 1 1 d . . . 
O41 O 0.3930(6) 0.4199(4) 0.6286(4) 0.037(2) Uani 1 1 d . . . 
O42 O 0.4130(6) 0.4122(4) 0.4979(4) 0.031(2) Uani 1 1 d . . . 
O43 O 0.4159(6) 0.3974(4) 0.3682(4) 0.035(2) Uani 1 1 d . . . 
O44 O 0.3844(5) 0.1898(4) 0.6302(4) 0.0262(19) Uani 1 1 d . . . 
O45 O 0.3933(6) 0.1876(4) 0.4985(4) 0.033(2) Uani 1 1 d . . . 
O46 O -0.1017(5) 0.2951(4) -0.1310(4) 0.036(2) Uani 1 1 d . . . 
O47 O 0.2097(6) -0.0046(3) 0.5442(4) 0.027(2) Uani 1 1 d . . . 
O48 O 0.2127(6) -0.0021(4) 0.3515(4) 0.031(2) 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 1.36(2) . ? 
C302 C303 1.48(2) . ? 
C303 C304 1.51(2) . ? 
C101 C102 1.334(17) . ? 
C101 C101 1.65(5) 3_566 ? 
C102 C103 1.473(19) . ? 
C103 C104 1.482(19) . ? 
Si1 O15 1.587(8) . ? 
Si1 O47 1.590(7) 2 ? 
Si1 O16 1.594(8) . ? 
Si1 O1 1.608(7) . ? 
Si2 O13 1.581(8) . ? 
Si2 O1 1.590(8) . ? 
Si2 O6 1.595(8) . ? 
Si2 O2 1.605(7) . ? 
Si3 O3 1.587(7) . ? 
Si3 O2 1.592(7) . ? 
Si3 O46 1.596(7) . ? 
Si3 O45 1.606(8) 4_565 ? 
Si4 O4 1.580(7) . ? 
Si4 O42 1.581(8) 4_565 ? 
Si4 O43 1.584(8) 4_565 ? 
Si4 O3 1.595(8) . ? 
Si5 O14 1.595(9) . ? 
Si5 O5 1.598(7) . ? 
Si5 O21 1.600(7) . ? 
Si5 O4 1.621(7) . ? 
Si6 O18 1.585(8) . ? 
Si6 O19 1.589(8) . ? 
Si6 O6 1.592(8) . ? 
Si6 O5 1.602(7) . ? 
Si7 O17 1.576(8) . ? 
Si7 O23 1.601(10) . ? 
Si7 O48 1.615(8) 2 ? 
Si7 O7 1.619(9) . ? 
Si8 O12 1.574(8) . ? 
Si8 O7 1.576(8) . ? 
Si8 O13 1.595(8) . ? 
Si8 O8 1.603(7) . ? 
Si9 O8 1.580(8) . ? 
Si9 O44 1.605(8) 4_565 ? 
Si9 O25 1.611(9) . ? 
Si9 O9 1.613(8) . ? 
Si10 O10 1.588(8) . ? 
Si10 O41 1.592(8) 4_565 ? 
Si10 O9 1.601(8) . ? 
Si10 O26 1.608(9) . ? 
Si11 O10 1.586(8) . ? 
Si11 O14 1.598(9) . ? 
Si11 O11 1.602(9) . ? 
Si11 O22 1.618(8) . ? 
Si12 O11 1.589(8) . ? 
Si12 O24 1.599(8) . ? 
Si12 O12 1.606(8) . ? 
Si12 O20 1.608(7) . ? 
Si13 O27 1.579(7) . ? 
Si13 O21 1.602(7) 2 ? 
Si13 O42 1.603(9) . ? 
Si13 O41 1.614(9) . ? 
Si14 O39 1.578(8) . ? 
Si14 O32 1.595(8) . ? 
Si14 O27 1.599(8) . ? 
Si14 O28 1.602(7) . ? 
Si15 O29 1.576(8) . ? 
Si15 O20 1.585(7) 4_566 ? 
Si15 O19 1.598(8) 4_566 ? 
Si15 O28 1.602(7) . ? 
Si16 O30 1.587(7) . ? 
Si16 O16 1.599(8) 4_566 ? 
Si16 O29 1.606(7) . ? 
Si16 O17 1.618(9) 4_566 ? 
Si17 O40 1.598(9) . ? 
Si17 O47 1.599(7) . ? 
Si17 O30 1.601(8) . ? 
Si17 O31 1.619(8) . ? 
Si18 O31 1.587(7) . ? 
Si18 O45 1.600(8) . ? 
Si18 O44 1.605(7) . ? 
Si18 O32 1.616(8) . ? 
Si19 O22 1.588(8) 2 ? 
Si19 O23 1.592(10) . ? 
Si19 O33 1.594(8) . ? 
Si19 O43 1.631(8) . ? 
Si20 O34 1.594(7) . ? 
Si20 O38 1.598(8) . ? 
Si20 O33 1.601(8) . ? 
Si20 O39 1.612(8) . ? 
Si21 O25 1.591(9) . ? 
Si21 O18 1.600(8) 4_566 ? 
Si21 O34 1.603(7) . ? 
Si21 O35 1.607(8) . ? 
Si22 O15 1.591(8) 4_566 ? 
Si22 O26 1.604(9) . ? 
Si22 O36 1.618(9) . ? 
Si22 O35 1.621(8) . ? 
Si23 O36 1.571(9) . ? 
Si23 O40 1.595(9) . ? 
Si23 O48 1.599(8) . ? 
Si23 O37 1.613(8) . ? 
Si24 O37 1.583(8) . ? 
Si24 O46 1.592(7) 4_666 ? 
Si24 O24 1.603(8) . ? 
Si24 O38 1.604(8) . ? 
O15 Si22 1.591(8) 4_665 ? 
O16 Si16 1.599(8) 4_665 ? 
O17 Si16 1.618(9) 4_665 ? 
O18 Si21 1.600(8) 4_665 ? 
O19 Si15 1.598(8) 4_665 ? 
O20 Si15 1.585(7) 4_665 ? 
O21 Si13 1.602(7) 2_545 ? 
O22 Si19 1.588(8) 2_545 ? 
O41 Si10 1.592(8) 4_666 ? 
O42 Si4 1.581(8) 4_666 ? 
O43 Si4 1.584(8) 4_666 ? 
O44 Si9 1.605(8) 4_666 ? 
O45 Si3 1.606(8) 4_666 ? 
O46 Si24 1.592(7) 4_565 ? 
O47 Si1 1.590(7) 2_545 ? 
O48 Si7 1.615(8) 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 
C301 C302 C303 126(4) . . ? 
C302 C303 C304 134(4) . . ? 
C102 C101 C101 157(4) . 3_566 ? 
C101 C102 C103 153(4) . . ? 
C102 C103 C104 141(4) . . ? 
O15 Si1 O47 111.0(4) . 2 ? 
O15 Si1 O16 109.9(5) . . ? 
O47 Si1 O16 110.2(5) 2 . ? 
O15 Si1 O1 108.3(5) . . ? 
O47 Si1 O1 107.6(4) 2 . ? 
O16 Si1 O1 109.8(5) . . ? 
O13 Si2 O1 109.5(5) . . ? 
O13 Si2 O6 107.7(5) . . ? 
O1 Si2 O6 111.1(4) . . ? 
O13 Si2 O2 109.6(4) . . ? 
O1 Si2 O2 107.9(4) . . ? 
O6 Si2 O2 111.0(5) . . ? 
O3 Si3 O2 112.0(4) . . ? 
O3 Si3 O46 108.2(5) . . ? 
O2 Si3 O46 109.4(4) . . ? 
O3 Si3 O45 109.1(5) . 4_565 ? 
O2 Si3 O45 109.1(4) . 4_565 ? 
O46 Si3 O45 109.1(4) . 4_565 ? 
O4 Si4 O42 109.9(5) . 4_565 ? 
O4 Si4 O43 107.7(5) . 4_565 ? 
O42 Si4 O43 110.9(5) 4_565 4_565 ? 
O4 Si4 O3 111.3(4) . . ? 
O42 Si4 O3 107.5(5) 4_565 . ? 
O43 Si4 O3 109.7(5) 4_565 . ? 
O14 Si5 O5 110.3(4) . . ? 
O14 Si5 O21 110.8(4) . . ? 
O5 Si5 O21 107.3(4) . . ? 
O14 Si5 O4 107.7(4) . . ? 
O5 Si5 O4 110.8(4) . . ? 
O21 Si5 O4 110.1(4) . . ? 
O18 Si6 O19 108.7(4) . . ? 
O18 Si6 O6 111.2(5) . . ? 
O19 Si6 O6 110.2(5) . . ? 
O18 Si6 O5 108.3(5) . . ? 
O19 Si6 O5 110.0(5) . . ? 
O6 Si6 O5 108.4(4) . . ? 
O17 Si7 O23 108.3(4) . . ? 
O17 Si7 O48 111.7(5) . 2 ? 
O23 Si7 O48 109.9(4) . 2 ? 
O17 Si7 O7 109.7(5) . . ? 
O23 Si7 O7 109.4(4) . . ? 
O48 Si7 O7 107.8(5) 2 . ? 
O12 Si8 O7 110.4(5) . . ? 
O12 Si8 O13 108.8(4) . . ? 
O7 Si8 O13 110.4(5) . . ? 
O12 Si8 O8 109.9(5) . . ? 
O7 Si8 O8 107.2(5) . . ? 
O13 Si8 O8 110.0(4) . . ? 
O8 Si9 O44 111.7(4) . 4_565 ? 
O8 Si9 O25 108.1(4) . . ? 
O44 Si9 O25 108.6(4) 4_565 . ? 
O8 Si9 O9 108.4(5) . . ? 
O44 Si9 O9 109.3(4) 4_565 . ? 
O25 Si9 O9 110.8(3) . . ? 
O10 Si10 O41 109.9(5) . 4_565 ? 
O10 Si10 O9 109.3(5) . . ? 
O41 Si10 O9 109.9(4) 4_565 . ? 
O10 Si10 O26 109.3(4) . . ? 
O41 Si10 O26 108.0(4) 4_565 . ? 
O9 Si10 O26 110.4(4) . . ? 
O10 Si11 O14 107.9(5) . . ? 
O10 Si11 O11 110.5(5) . . ? 
O14 Si11 O11 109.5(4) . . ? 
O10 Si11 O22 109.2(5) . . ? 
O14 Si11 O22 110.3(4) . . ? 
O11 Si11 O22 109.4(5) . . ? 
O11 Si12 O24 111.4(4) . . ? 
O11 Si12 O12 107.6(5) . . ? 
O24 Si12 O12 111.5(4) . . ? 
O11 Si12 O20 110.7(5) . . ? 
O24 Si12 O20 107.0(4) . . ? 
O12 Si12 O20 108.5(4) . . ? 
O27 Si13 O21 110.5(4) . 2 ? 
O27 Si13 O42 109.2(5) . . ? 
O21 Si13 O42 109.1(4) 2 . ? 
O27 Si13 O41 111.1(5) . . ? 
O21 Si13 O41 107.4(4) 2 . ? 
O42 Si13 O41 109.4(5) . . ? 
O39 Si14 O32 108.9(5) . . ? 
O39 Si14 O27 110.5(5) . . ? 
O32 Si14 O27 108.2(4) . . ? 
O39 Si14 O28 111.1(4) . . ? 
O32 Si14 O28 108.9(4) . . ? 
O27 Si14 O28 109.1(4) . . ? 
O29 Si15 O20 110.0(5) . 4_566 ? 
O29 Si15 O19 109.2(5) . 4_566 ? 
O20 Si15 O19 110.3(4) 4_566 4_566 ? 
O29 Si15 O28 109.3(4) . . ? 
O20 Si15 O28 108.3(4) 4_566 . ? 
O19 Si15 O28 109.8(5) 4_566 . ? 
O30 Si16 O16 110.6(5) . 4_566 ? 
O30 Si16 O29 109.2(4) . . ? 
O16 Si16 O29 110.4(5) 4_566 . ? 
O30 Si16 O17 108.6(5) . 4_566 ? 
O16 Si16 O17 108.3(5) 4_566 4_566 ? 
O29 Si16 O17 109.7(5) . 4_566 ? 
O40 Si17 O47 110.1(4) . . ? 
O40 Si17 O30 110.1(5) . . ? 
O47 Si17 O30 109.0(4) . . ? 
O40 Si17 O31 109.4(4) . . ? 
O47 Si17 O31 109.0(5) . . ? 
O30 Si17 O31 109.2(5) . . ? 
O31 Si18 O45 109.9(5) . . ? 
O31 Si18 O44 106.4(4) . . ? 
O45 Si18 O44 110.3(4) . . ? 
O31 Si18 O32 110.1(4) . . ? 
O45 Si18 O32 110.3(5) . . ? 
O44 Si18 O32 109.8(5) . . ? 
O22 Si19 O23 110.4(4) 2 . ? 
O22 Si19 O33 107.5(5) 2 . ? 
O23 Si19 O33 110.8(4) . . ? 
O22 Si19 O43 109.1(5) 2 . ? 
O23 Si19 O43 107.2(4) . . ? 
O33 Si19 O43 111.8(5) . . ? 
O34 Si20 O38 109.4(4) . . ? 
O34 Si20 O33 109.1(4) . . ? 
O38 Si20 O33 110.5(4) . . ? 
O34 Si20 O39 110.2(4) . . ? 
O38 Si20 O39 108.6(5) . . ? 
O33 Si20 O39 109.2(5) . . ? 
O25 Si21 O18 108.0(4) . 4_566 ? 
O25 Si21 O34 111.5(4) . . ? 
O18 Si21 O34 108.9(4) 4_566 . ? 
O25 Si21 O35 109.9(4) . . ? 
O18 Si21 O35 110.6(5) 4_566 . ? 
O34 Si21 O35 108.0(4) . . ? 
O15 Si22 O26 108.4(4) 4_566 . ? 
O15 Si22 O36 110.0(5) 4_566 . ? 
O26 Si22 O36 110.1(4) . . ? 
O15 Si22 O35 109.1(4) 4_566 . ? 
O26 Si22 O35 110.7(4) . . ? 
O36 Si22 O35 108.5(5) . . ? 
O36 Si23 O40 110.2(5) . . ? 
O36 Si23 O48 108.9(5) . . ? 
O40 Si23 O48 110.1(5) . . ? 
O36 Si23 O37 111.8(5) . . ? 
O40 Si23 O37 109.0(4) . . ? 
O48 Si23 O37 106.8(5) . . ? 
O37 Si24 O46 112.4(5) . 4_666 ? 
O37 Si24 O24 109.2(4) . . ? 
O46 Si24 O24 107.8(4) 4_666 . ? 
O37 Si24 O38 109.7(5) . . ? 
O46 Si24 O38 109.8(5) 4_666 . ? 
O24 Si24 O38 107.9(4) . . ? 
Si2 O1 Si1 147.2(6) . . ? 
Si3 O2 Si2 147.3(5) . . ? 
Si3 O3 Si4 164.3(6) . . ? 
Si4 O4 Si5 149.9(6) . . ? 
Si5 O5 Si6 148.6(5) . . ? 
Si6 O6 Si2 163.9(6) . . ? 
Si8 O7 Si7 157.2(7) . . ? 
Si9 O8 Si8 154.0(6) . . ? 
Si10 O9 Si9 151.4(5) . . ? 
Si11 O10 Si10 157.1(6) . . ? 
Si12 O11 Si11 156.9(6) . . ? 
Si8 O12 Si12 170.1(6) . . ? 
Si2 O13 Si8 164.5(6) . . ? 
Si5 O14 Si11 159.8(5) . . ? 
Si1 O15 Si22 150.7(6) . 4_665 ? 
Si1 O16 Si16 177.1(7) . 4_665 ? 
Si7 O17 Si16 148.5(6) . 4_665 ? 
Si6 O18 Si21 143.0(6) . 4_665 ? 
Si6 O19 Si15 168.3(6) . 4_665 ? 
Si15 O20 Si12 144.2(5) 4_665 . ? 
Si5 O21 Si13 146.6(5) . 2_545 ? 
Si19 O22 Si11 151.6(6) 2_545 . ? 
Si19 O23 Si7 155.4(4) . . ? 
Si12 O24 Si24 149.2(4) . . ? 
Si21 O25 Si9 151.9(4) . . ? 
Si22 O26 Si10 145.3(4) . . ? 
Si13 O27 Si14 156.0(6) . . ? 
Si15 O28 Si14 149.2(5) . . ? 
Si15 O29 Si16 163.9(5) . . ? 
Si16 O30 Si17 158.2(6) . . ? 
Si18 O31 Si17 147.6(5) . . ? 
Si14 O32 Si18 157.5(6) . . ? 
Si19 O33 Si20 151.7(6) . . ? 
Si20 O34 Si21 148.5(5) . . ? 
Si21 O35 Si22 151.4(5) . . ? 
Si23 O36 Si22 160.2(6) . . ? 
Si24 O37 Si23 152.2(6) . . ? 
Si20 O38 Si24 156.2(6) . . ? 
Si14 O39 Si20 167.4(6) . . ? 
Si23 O40 Si17 162.5(5) . . ? 
Si10 O41 Si13 149.1(6) 4_666 . ? 
Si4 O42 Si13 160.8(6) 4_666 . ? 
Si4 O43 Si19 148.7(6) 4_666 . ? 
Si9 O44 Si18 149.0(6) 4_666 . ? 
Si18 O45 Si3 155.6(6) . 4_666 ? 
Si24 O46 Si3 155.4(6) 4_565 . ? 
Si1 O47 Si17 149.0(6) 2_545 . ? 
Si23 O48 Si7 146.8(6) . 2_545 ? 
  
_diffrn_measured_fraction_theta_max    0.947 
_diffrn_reflns_theta_full              28.71 
_diffrn_measured_fraction_theta_full   0.947 
_refine_diff_density_max    0.641 
_refine_diff_density_min   -0.565 
_refine_diff_density_rms    0.134 




  
data_f_2butyne_3_2_mo 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C1 O48 Si24' 
_chemical_formula_weight          1454 
  
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                    13.375(17) 
_cell_length_b                    20.13(2) 
_cell_length_c                    19.90(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.10(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      5358(11) 
_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           0.06 
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.855 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3000 
_exptl_absorpt_coefficient_mu     0.676 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   0.8596 
_exptl_absorpt_correction_T_max   0.9593 
_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             61691 
_diffrn_reflns_av_R_equivalents   0.0941 
_diffrn_reflns_av_sigmaI/netI     0.1146 
_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        -25 
_diffrn_reflns_limit_l_max        26 
_diffrn_reflns_theta_min          1.01 
_diffrn_reflns_theta_max          28.54 
_reflns_number_total              12810 
_reflns_number_gt                 6505 
_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)+(0.0488P)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          12810 
_refine_ls_number_parameters      661 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1164 
_refine_ls_R_factor_gt            0.0534 
_refine_ls_wR_factor_ref          0.1280 
_refine_ls_wR_factor_gt           0.1119 
_refine_ls_goodness_of_fit_ref    0.862 
_refine_ls_restrained_S_all       0.862 
_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 1.007(4) 0.488(3) 0.455(3) 0.16(3) Uiso 0.244(14) 1 d PG . 1 
C102 C 0.993(3) 0.4957(19) 0.382(3) 0.46(9) Uiso 0.244(14) 1 d PG . 1 
C103 C 0.982(4) 0.502(2) 0.322(3) 0.61(14) Uiso 0.244(14) 1 d PG . 1 
C104 C 0.968(6) 0.509(4) 0.250(3) 0.42(7) Uiso 0.244(14) 1 d PG . 1 
Si1 Si 0.32202(14) 0.42060(8) -0.05578(10) 0.0147(4) Uani 1 1 d . . . 
Si2 Si 0.16734(15) 0.31311(9) -0.03033(9) 0.0171(4) Uani 1 1 d . . . 
Si3 Si -0.05011(14) 0.27965(9) -0.06247(10) 0.0169(4) Uani 1 1 d . . . 
Si4 Si -0.03560(14) 0.12373(9) -0.06261(10) 0.0156(4) Uani 1 1 d . . . 
Si5 Si 0.17750(15) 0.07628(9) -0.02801(9) 0.0148(4) Uani 1 1 d . . . 
Si6 Si 0.31576(14) 0.19463(9) -0.05586(10) 0.0162(4) Uani 1 1 d . . . 
Si7 Si 0.32036(15) 0.42504(9) 0.17151(9) 0.0151(4) Uani 1 1 d . . . 
Si8 Si 0.17552(14) 0.31127(9) 0.12682(9) 0.0164(4) Uani 1 1 d . . . 
Si9 Si -0.03548(15) 0.27323(9) 0.17572(9) 0.0152(4) Uani 1 1 d . . . 
Si10 Si -0.03308(15) 0.11934(9) 0.17586(9) 0.0156(4) Uani 1 1 d . . . 
Si11 Si 0.17674(15) 0.07133(9) 0.12925(10) 0.0160(4) Uani 1 1 d . . . 
Si12 Si 0.31532(15) 0.19008(9) 0.16612(9) 0.0163(4) Uani 1 1 d . . . 
Si13 Si 0.33493(14) 0.42782(8) 0.55729(11) 0.0151(4) Uani 1 1 d . . . 
Si14 Si 0.18870(15) 0.31189(10) 0.52730(9) 0.0171(4) Uani 1 1 d . . . 
Si15 Si -0.02927(14) 0.27745(9) 0.56116(10) 0.0153(4) Uani 1 1 d . . . 
Si16 Si -0.03283(14) 0.12164(9) 0.56407(10) 0.0156(4) Uani 1 1 d . . . 
Si17 Si 0.17974(15) 0.07066(9) 0.52721(9) 0.0138(4) Uani 1 1 d . . . 
Si18 Si 0.31859(15) 0.18687(8) 0.56231(10) 0.0156(4) Uani 1 1 d . . . 
Si19 Si 0.31584(15) 0.42366(9) 0.32794(9) 0.0156(4) Uani 1 1 d . . . 
Si20 Si 0.17116(14) 0.31219(9) 0.36914(10) 0.0168(4) Uani 1 1 d . . . 
Si21 Si -0.04330(15) 0.27339(9) 0.33101(9) 0.0164(4) Uani 1 1 d . . . 
Si22 Si -0.03695(15) 0.11879(9) 0.32965(9) 0.0166(4) Uani 1 1 d . . . 
Si23 Si 0.17787(15) 0.07213(8) 0.36926(10) 0.0156(4) Uani 1 1 d . . . 
Si24 Si 0.30077(14) 0.19328(9) 0.32021(9) 0.0161(4) Uani 1 1 d . . . 
O1 O 0.2235(3) 0.3769(2) -0.0578(3) 0.0318(12) Uani 1 1 d . . . 
O2 O 0.0595(3) 0.3098(2) -0.0659(2) 0.0240(11) Uani 1 1 d . . . 
O3 O -0.0446(4) 0.2017(2) -0.0494(3) 0.0408(13) Uani 1 1 d . . . 
O4 O 0.0797(3) 0.1037(2) -0.0669(2) 0.0263(12) Uani 1 1 d . . . 
O5 O 0.2709(3) 0.1217(2) -0.0455(3) 0.0269(12) Uani 1 1 d . . . 
O6 O 0.2275(3) 0.2472(2) -0.0470(3) 0.0358(13) Uani 1 1 d . . . 
O7 O 0.2298(4) 0.3760(3) 0.1542(3) 0.0389(15) Uani 1 1 d . . . 
O8 O 0.0704(4) 0.3048(2) 0.1658(2) 0.0350(13) Uani 1 1 d . . . 
O9 O -0.0316(4) 0.1961(2) 0.1558(2) 0.0296(13) Uani 1 1 d . . . 
O10 O 0.0766(4) 0.0892(2) 0.1687(2) 0.0332(13) Uani 1 1 d . . . 
O11 O 0.2652(4) 0.1208(2) 0.1512(2) 0.0340(14) Uani 1 1 d . . . 
O12 O 0.2438(4) 0.2481(2) 0.1385(2) 0.0365(14) Uani 1 1 d . . . 
O13 O 0.1544(4) 0.3185(2) 0.0485(2) 0.0430(14) Uani 1 1 d . . . 
O14 O 0.1568(3) 0.0782(2) 0.0506(2) 0.0289(12) Uani 1 1 d . . . 
O15 O 0.3776(4) 0.4138(2) -0.1251(2) 0.0316(13) Uani 1 1 d . . . 
O16 O 0.3925(4) 0.3945(3) 0.0046(2) 0.0419(15) Uani 1 1 d . . . 
O17 O 0.4195(3) 0.4015(2) 0.1336(2) 0.0255(12) Uani 1 1 d . . . 
O18 O 0.3612(3) 0.2001(2) -0.1301(2) 0.0249(11) Uani 1 1 d . . . 
O19 O 0.4021(4) 0.2083(3) -0.0025(2) 0.0356(14) Uani 1 1 d . . . 
O20 O 0.4200(3) 0.1953(2) 0.1283(2) 0.0284(12) Uani 1 1 d . . . 
O21 O 0.2039(3) 0.00247(19) -0.0518(2) 0.0244(11) Uani 1 1 d . . . 
O22 O 0.2096(4) -0.0028(2) 0.1479(2) 0.0277(13) Uani 1 1 d . . . 
O23 O 0.3432(3) 0.42356(19) 0.2508(3) 0.0318(10) Uani 1 1 d . . . 
O24 O 0.3379(3) 0.19818(19) 0.2442(2) 0.0282(10) Uani 1 1 d . . . 
O25 O -0.0658(3) 0.28235(17) 0.2524(3) 0.0241(10) Uani 1 1 d . . . 
O26 O -0.0678(3) 0.11025(17) 0.2523(3) 0.0235(10) Uani 1 1 d . . . 
O27 O 0.2426(3) 0.3780(2) 0.5521(3) 0.0378(14) Uani 1 1 d . . . 
O28 O 0.0741(3) 0.3138(2) 0.5528(3) 0.0293(12) Uani 1 1 d . . . 
O29 O -0.0112(4) 0.1992(2) 0.5664(2) 0.0383(13) Uani 1 1 d . . . 
O30 O 0.0684(3) 0.0827(2) 0.5541(3) 0.0323(12) Uani 1 1 d . . . 
O31 O 0.2561(3) 0.1199(2) 0.5650(2) 0.0260(12) Uani 1 1 d . . . 
O32 O 0.2454(3) 0.2491(2) 0.5598(3) 0.0317(12) Uani 1 1 d . . . 
O33 O 0.2209(4) 0.3789(2) 0.3417(3) 0.0300(13) Uani 1 1 d . . . 
O34 O 0.0546(4) 0.3143(2) 0.3543(2) 0.0270(12) Uani 1 1 d . . . 
O35 O -0.0251(4) 0.1959(2) 0.3480(2) 0.0287(13) Uani 1 1 d . . . 
O36 O 0.0668(4) 0.0835(3) 0.3437(3) 0.0404(15) Uani 1 1 d . . . 
O37 O 0.2537(4) 0.1221(2) 0.3331(2) 0.0342(14) Uani 1 1 d . . . 
O38 O 0.2187(4) 0.2486(2) 0.3319(2) 0.0329(13) Uani 1 1 d . . . 
O39 O 0.1921(4) 0.3052(3) 0.4480(2) 0.0461(14) Uani 1 1 d . . . 
O40 O 0.1829(4) 0.0847(2) 0.4484(2) 0.0353(13) Uani 1 1 d . . . 
O41 O 0.3899(4) 0.4191(2) 0.6287(3) 0.0328(14) Uani 1 1 d . . . 
O42 O 0.4130(4) 0.4142(2) 0.4987(2) 0.0301(12) Uani 1 1 d . . . 
O43 O 0.4100(4) 0.3949(2) 0.3678(2) 0.0285(12) Uani 1 1 d . . . 
O44 O 0.3853(3) 0.1895(2) 0.6292(2) 0.0256(11) Uani 1 1 d . . . 
O45 O 0.3901(4) 0.1864(2) 0.4971(2) 0.0330(13) Uani 1 1 d . . . 
O46 O -0.1050(4) 0.2943(3) -0.1315(2) 0.0412(15) Uani 1 1 d . . . 
O47 O 0.2092(3) -0.0045(2) 0.5433(2) 0.0251(12) Uani 1 1 d . . . 
O48 O 0.2112(4) -0.0016(2) 0.3520(2) 0.0314(13) 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 1.4598 . ? 
C101 C101 1.87(10) 3_766 ? 
C102 C103 1.2099 . ? 
C103 C104 1.4598 . ? 
Si1 O15 1.575(5) . ? 
Si1 O47 1.584(5) 2 ? 
Si1 O1 1.586(5) . ? 
Si1 O16 1.614(5) . ? 
Si2 O13 1.583(5) . ? 
Si2 O1 1.584(5) . ? 
Si2 O6 1.587(5) . ? 
Si2 O2 1.607(5) . ? 
Si3 O46 1.584(5) . ? 
Si3 O45 1.586(5) 4_565 ? 
Si3 O2 1.589(5) . ? 
Si3 O3 1.593(5) . ? 
Si4 O3 1.595(5) . ? 
Si4 O42 1.595(5) 4_565 ? 
Si4 O4 1.596(5) . ? 
Si4 O43 1.607(5) 4_565 ? 
Si5 O5 1.586(5) . ? 
Si5 O14 1.589(5) . ? 
Si5 O21 1.599(4) . ? 
Si5 O4 1.616(5) . ? 
Si6 O19 1.592(5) . ? 
Si6 O6 1.595(5) . ? 
Si6 O5 1.600(5) . ? 
Si6 O18 1.603(5) . ? 
Si7 O17 1.599(5) . ? 
Si7 O7 1.600(5) . ? 
Si7 O48 1.604(5) 2 ? 
Si7 O23 1.607(6) . ? 
Si8 O12 1.583(5) . ? 
Si8 O7 1.587(5) . ? 
Si8 O13 1.590(5) . ? 
Si8 O8 1.612(5) . ? 
Si9 O8 1.565(5) . ? 
Si9 O25 1.589(5) . ? 
Si9 O44 1.593(5) 4_565 ? 
Si9 O9 1.602(5) . ? 
Si10 O41 1.593(5) 4_565 ? 
Si10 O10 1.594(5) . ? 
Si10 O9 1.597(5) . ? 
Si10 O26 1.602(5) . ? 
Si11 O14 1.593(5) . ? 
Si11 O10 1.595(5) . ? 
Si11 O22 1.599(5) . ? 
Si11 O11 1.607(5) . ? 
Si12 O11 1.575(5) . ? 
Si12 O24 1.590(5) . ? 
Si12 O20 1.594(5) . ? 
Si12 O12 1.606(5) . ? 
Si13 O42 1.591(5) . ? 
Si13 O21 1.594(4) 2 ? 
Si13 O27 1.594(5) . ? 
Si13 O41 1.609(5) . ? 
Si14 O39 1.585(5) . ? 
Si14 O27 1.592(5) . ? 
Si14 O32 1.609(5) . ? 
Si14 O28 1.616(5) . ? 
Si15 O28 1.573(5) . ? 
Si15 O19 1.589(5) 4_566 ? 
Si15 O20 1.596(5) 4_566 ? 
Si15 O29 1.597(5) . ? 
Si16 O30 1.577(5) . ? 
Si16 O16 1.581(5) 4_566 ? 
Si16 O29 1.588(5) . ? 
Si16 O17 1.593(5) 4_566 ? 
Si17 O40 1.595(5) . ? 
Si17 O47 1.596(5) . ? 
Si17 O30 1.602(5) . ? 
Si17 O31 1.609(5) . ? 
Si18 O31 1.587(5) . ? 
Si18 O32 1.591(5) . ? 
Si18 O44 1.603(5) . ? 
Si18 O45 1.613(5) . ? 
Si19 O23 1.579(6) . ? 
Si19 O33 1.582(5) . ? 
Si19 O22 1.593(5) 2 ? 
Si19 O43 1.596(5) . ? 
Si20 O34 1.587(5) . ? 
Si20 O33 1.594(5) . ? 
Si20 O39 1.599(5) . ? 
Si20 O38 1.611(5) . ? 
Si21 O18 1.587(5) 4_566 ? 
Si21 O25 1.604(5) . ? 
Si21 O35 1.614(5) . ? 
Si21 O34 1.614(5) . ? 
Si22 O36 1.583(6) . ? 
Si22 O15 1.597(5) 4_566 ? 
Si22 O26 1.601(6) . ? 
Si22 O35 1.603(5) . ? 
Si23 O36 1.587(6) . ? 
Si23 O48 1.588(5) . ? 
Si23 O40 1.596(5) . ? 
Si23 O37 1.601(5) . ? 
Si24 O38 1.580(5) . ? 
Si24 O37 1.586(5) . ? 
Si24 O24 1.597(5) . ? 
Si24 O46 1.603(5) 4_666 ? 
O15 Si22 1.597(5) 4_665 ? 
O16 Si16 1.581(5) 4_665 ? 
O17 Si16 1.593(5) 4_665 ? 
O18 Si21 1.587(5) 4_665 ? 
O19 Si15 1.589(5) 4_665 ? 
O20 Si15 1.597(5) 4_665 ? 
O21 Si13 1.594(4) 2_545 ? 
O22 Si19 1.593(5) 2_545 ? 
O41 Si10 1.593(5) 4_666 ? 
O42 Si4 1.595(5) 4_666 ? 
O43 Si4 1.607(5) 4_666 ? 
O44 Si9 1.593(5) 4_666 ? 
O45 Si3 1.586(5) 4_666 ? 
O46 Si24 1.603(5) 4_565 ? 
O47 Si1 1.584(5) 2_545 ? 
O48 Si7 1.604(5) 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 
C102 C101 C101 156(5) . 3_766 ? 
C103 C102 C101 180.00(5) . . ? 
C102 C103 C104 180.0 . . ? 
O15 Si1 O47 110.1(3) . 2 ? 
O15 Si1 O1 108.9(3) . . ? 
O47 Si1 O1 108.2(3) 2 . ? 
O15 Si1 O16 110.4(3) . . ? 
O47 Si1 O16 110.4(3) 2 . ? 
O1 Si1 O16 108.8(3) . . ? 
O13 Si2 O1 109.8(3) . . ? 
O13 Si2 O6 108.7(3) . . ? 
O1 Si2 O6 111.4(3) . . ? 
O13 Si2 O2 109.9(3) . . ? 
O1 Si2 O2 107.9(3) . . ? 
O6 Si2 O2 109.2(3) . . ? 
O46 Si3 O45 109.5(3) . 4_565 ? 
O46 Si3 O2 108.5(3) . . ? 
O45 Si3 O2 109.5(3) 4_565 . ? 
O46 Si3 O3 110.3(3) . . ? 
O45 Si3 O3 109.0(3) 4_565 . ? 
O2 Si3 O3 110.0(3) . . ? 
O3 Si4 O42 108.2(3) . 4_565 ? 
O3 Si4 O4 109.3(3) . . ? 
O42 Si4 O4 109.7(3) 4_565 . ? 
O3 Si4 O43 109.7(3) . 4_565 ? 
O42 Si4 O43 110.6(3) 4_565 4_565 ? 
O4 Si4 O43 109.3(3) . 4_565 ? 
O5 Si5 O14 109.9(3) . . ? 
O5 Si5 O21 107.2(3) . . ? 
O14 Si5 O21 110.6(3) . . ? 
O5 Si5 O4 109.6(3) . . ? 
O14 Si5 O4 108.7(3) . . ? 
O21 Si5 O4 110.8(3) . . ? 
O19 Si6 O6 110.4(3) . . ? 
O19 Si6 O5 110.1(3) . . ? 
O6 Si6 O5 108.5(3) . . ? 
O19 Si6 O18 109.1(3) . . ? 
O6 Si6 O18 109.7(3) . . ? 
O5 Si6 O18 109.0(3) . . ? 
O17 Si7 O7 110.1(3) . . ? 
O17 Si7 O48 110.7(3) . 2 ? 
O7 Si7 O48 107.8(3) . 2 ? 
O17 Si7 O23 107.6(3) . . ? 
O7 Si7 O23 110.0(3) . . ? 
O48 Si7 O23 110.7(3) 2 . ? 
O12 Si8 O7 110.2(3) . . ? 
O12 Si8 O13 108.6(3) . . ? 
O7 Si8 O13 110.0(3) . . ? 
O12 Si8 O8 111.6(3) . . ? 
O7 Si8 O8 107.5(3) . . ? 
O13 Si8 O8 109.0(3) . . ? 
O8 Si9 O25 107.9(3) . . ? 
O8 Si9 O44 109.7(3) . 4_565 ? 
O25 Si9 O44 109.4(3) . 4_565 ? 
O8 Si9 O9 109.4(3) . . ? 
O25 Si9 O9 110.9(2) . . ? 
O44 Si9 O9 109.5(3) 4_565 . ? 
O41 Si10 O10 110.9(3) 4_565 . ? 
O41 Si10 O9 109.4(3) 4_565 . ? 
O10 Si10 O9 109.5(3) . . ? 
O41 Si10 O26 108.4(3) 4_565 . ? 
O10 Si10 O26 108.0(3) . . ? 
O9 Si10 O26 110.6(2) . . ? 
O14 Si11 O10 109.0(3) . . ? 
O14 Si11 O22 110.7(3) . . ? 
O10 Si11 O22 109.1(3) . . ? 
O14 Si11 O11 109.6(3) . . ? 
O10 Si11 O11 110.1(3) . . ? 
O22 Si11 O11 108.3(3) . . ? 
O11 Si12 O24 110.8(3) . . ? 
O11 Si12 O20 110.1(3) . . ? 
O24 Si12 O20 106.8(3) . . ? 
O11 Si12 O12 109.0(3) . . ? 
O24 Si12 O12 111.8(3) . . ? 
O20 Si12 O12 108.2(3) . . ? 
O42 Si13 O21 109.0(3) . 2 ? 
O42 Si13 O27 110.8(3) . . ? 
O21 Si13 O27 109.6(3) 2 . ? 
O42 Si13 O41 109.3(3) . . ? 
O21 Si13 O41 108.2(3) 2 . ? 
O27 Si13 O41 110.0(3) . . ? 
O39 Si14 O27 111.5(3) . . ? 
O39 Si14 O32 108.6(3) . . ? 
O27 Si14 O32 108.6(3) . . ? 
O39 Si14 O28 110.1(3) . . ? 
O27 Si14 O28 108.2(3) . . ? 
O32 Si14 O28 109.8(3) . . ? 
O28 Si15 O19 109.8(3) . 4_566 ? 
O28 Si15 O20 107.7(3) . 4_566 ? 
O19 Si15 O20 111.0(3) 4_566 4_566 ? 
O28 Si15 O29 109.4(3) . . ? 
O19 Si15 O29 108.5(3) 4_566 . ? 
O20 Si15 O29 110.4(3) 4_566 . ? 
O30 Si16 O16 110.2(3) . 4_566 ? 
O30 Si16 O29 109.6(3) . . ? 
O16 Si16 O29 109.8(3) 4_566 . ? 
O30 Si16 O17 108.0(3) . 4_566 ? 
O16 Si16 O17 109.7(3) 4_566 4_566 ? 
O29 Si16 O17 109.5(3) . 4_566 ? 
O40 Si17 O47 111.1(3) . . ? 
O40 Si17 O30 109.1(3) . . ? 
O47 Si17 O30 107.8(3) . . ? 
O40 Si17 O31 109.4(3) . . ? 
O47 Si17 O31 109.5(3) . . ? 
O30 Si17 O31 109.9(3) . . ? 
O31 Si18 O32 110.3(3) . . ? 
O31 Si18 O44 107.0(3) . . ? 
O32 Si18 O44 110.0(3) . . ? 
O31 Si18 O45 109.6(3) . . ? 
O32 Si18 O45 110.2(3) . . ? 
O44 Si18 O45 109.8(3) . . ? 
O23 Si19 O33 110.8(3) . . ? 
O23 Si19 O22 110.1(3) . 2 ? 
O33 Si19 O22 107.8(3) . 2 ? 
O23 Si19 O43 107.4(3) . . ? 
O33 Si19 O43 109.9(3) . . ? 
O22 Si19 O43 110.9(3) 2 . ? 
O34 Si20 O33 108.9(3) . . ? 
O34 Si20 O39 110.9(3) . . ? 
O33 Si20 O39 109.7(3) . . ? 
O34 Si20 O38 108.9(3) . . ? 
O33 Si20 O38 110.3(3) . . ? 
O39 Si20 O38 108.2(3) . . ? 
O18 Si21 O25 106.8(3) 4_566 . ? 
O18 Si21 O35 110.1(3) 4_566 . ? 
O25 Si21 O35 110.0(2) . . ? 
O18 Si21 O34 110.0(3) 4_566 . ? 
O25 Si21 O34 111.9(2) . . ? 
O35 Si21 O34 108.1(3) . . ? 
O36 Si22 O15 110.1(3) . 4_566 ? 
O36 Si22 O26 110.2(3) . . ? 
O15 Si22 O26 108.3(3) 4_566 . ? 
O36 Si22 O35 108.0(3) . . ? 
O15 Si22 O35 109.9(3) 4_566 . ? 
O26 Si22 O35 110.4(2) . . ? 
O36 Si23 O48 109.2(3) . . ? 
O36 Si23 O40 109.3(3) . . ? 
O48 Si23 O40 110.5(3) . . ? 
O36 Si23 O37 111.0(3) . . ? 
O48 Si23 O37 108.2(3) . . ? 
O40 Si23 O37 108.5(3) . . ? 
O38 Si24 O37 109.6(3) . . ? 
O38 Si24 O24 108.3(3) . . ? 
O37 Si24 O24 109.5(2) . . ? 
O38 Si24 O46 110.3(3) . 4_666 ? 
O37 Si24 O46 110.8(3) . 4_666 ? 
O24 Si24 O46 108.2(3) . 4_666 ? 
Si2 O1 Si1 146.7(4) . . ? 
Si3 O2 Si2 145.5(3) . . ? 
Si3 O3 Si4 161.1(4) . . ? 
Si4 O4 Si5 147.3(3) . . ? 
Si5 O5 Si6 148.5(3) . . ? 
Si2 O6 Si6 162.4(4) . . ? 
Si8 O7 Si7 157.8(4) . . ? 
Si9 O8 Si8 152.1(3) . . ? 
Si10 O9 Si9 151.1(3) . . ? 
Si10 O10 Si11 154.6(4) . . ? 
Si12 O11 Si11 156.0(4) . . ? 
Si8 O12 Si12 167.9(4) . . ? 
Si2 O13 Si8 161.1(4) . . ? 
Si5 O14 Si11 159.3(3) . . ? 
Si1 O15 Si22 150.3(4) . 4_665 ? 
Si16 O16 Si1 172.5(4) 4_665 . ? 
Si16 O17 Si7 146.1(3) 4_665 . ? 
Si21 O18 Si6 141.2(3) 4_665 . ? 
Si15 O19 Si6 168.7(4) 4_665 . ? 
Si12 O20 Si15 142.5(3) . 4_665 ? 
Si13 O21 Si5 145.5(3) 2_545 . ? 
Si19 O22 Si11 151.4(4) 2_545 . ? 
Si19 O23 Si7 155.6(3) . . ? 
Si12 O24 Si24 149.4(3) . . ? 
Si9 O25 Si21 151.2(3) . . ? 
Si22 O26 Si10 145.7(3) . . ? 
Si14 O27 Si13 153.7(4) . . ? 
Si15 O28 Si14 148.9(3) . . ? 
Si16 O29 Si15 160.1(4) . . ? 
Si16 O30 Si17 156.4(3) . . ? 
Si18 O31 Si17 147.3(3) . . ? 
Si18 O32 Si14 157.1(4) . . ? 
Si19 O33 Si20 151.0(4) . . ? 
Si20 O34 Si21 146.8(3) . . ? 
Si22 O35 Si21 150.8(3) . . ? 
Si22 O36 Si23 160.3(4) . . ? 
Si24 O37 Si23 153.2(4) . . ? 
Si24 O38 Si20 154.4(4) . . ? 
Si14 O39 Si20 164.6(4) . . ? 
Si17 O40 Si23 160.2(3) . . ? 
Si10 O41 Si13 150.1(3) 4_666 . ? 
Si13 O42 Si4 157.9(4) . 4_666 ? 
Si19 O43 Si4 150.3(3) . 4_666 ? 
Si9 O44 Si18 150.1(3) 4_666 . ? 
Si3 O45 Si18 154.1(4) 4_666 . ? 
Si3 O46 Si24 155.7(4) . 4_565 ? 
Si1 O47 Si17 150.3(3) 2_545 . ? 
Si23 O48 Si7 148.1(4) . 2_545 ? 
  
_diffrn_measured_fraction_theta_max    0.941 
_diffrn_reflns_theta_full              28.54 
_diffrn_measured_fraction_theta_full   0.941 
_refine_diff_density_max    0.579 
_refine_diff_density_min   -0.597 
_refine_diff_density_rms    0.135 





  
data_f_c2butene_twin_02atm_1h 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C3 H0 O48 Si24' 
_chemical_formula_weight          1479 
  
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(6) 
_cell_length_b                    20.160(9) 
_cell_length_c                    19.990(9) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  89.983(8) 
_cell_angle_gamma                 90.00 
_cell_volume                      5426(4) 
_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           0.11 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.834 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3008 
_exptl_absorpt_coefficient_mu     0.667 
_exptl_absorpt_correction_type    Analytical 
_exptl_absorpt_correction_T_min   0.8973 
_exptl_absorpt_correction_T_max   0.9517 
_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             63454 
_diffrn_reflns_av_R_equivalents   0.0813 
_diffrn_reflns_av_sigmaI/netI     0.0933 
_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        -25 
_diffrn_reflns_limit_l_max        25 
_diffrn_reflns_theta_min          1.01 
_diffrn_reflns_theta_max          28.66 
_reflns_number_total              13037 
_reflns_number_gt                 5784 
_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)+(0.0727P)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          13037 
_refine_ls_number_parameters      666 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1217 
_refine_ls_R_factor_gt            0.0484 
_refine_ls_wR_factor_ref          0.1605 
_refine_ls_wR_factor_gt           0.1365 
_refine_ls_goodness_of_fit_ref    0.874 
_refine_ls_restrained_S_all       0.874 
_refine_ls_shift/su_max           0.083 
_refine_ls_shift/su_mean          0.007 
  
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 0.4450(18) -0.0203(13) 1.0348(9) 0.017(8) Uiso 0.202(7) 1 d PG . 1 
C102 C 0.5300(16) 0.0196(12) 1.0071(9) 0.028(9) Uiso 0.202(7) 1 d PG . 1 
C103 C 0.5490(13) 0.0294(12) 0.9417(10) 0.030(9) Uiso 0.202(7) 1 d PG . 1 
C104 C 0.4886(16) 0.0020(11) 0.8847(9) 0.14(3) Uiso 0.202(7) 1 d PG . 1 
C301 C 0.1946(15) 0.2592(8) 0.7691(14) 0.29(2) Uiso 0.560(12) 1 d PG A 2 
C302 C 0.0999(12) 0.2237(10) 0.7512(14) 0.148(10) Uiso 0.560(12) 1 d PG A 2 
C303 C 0.0915(12) 0.1583(10) 0.7393(14) 0.208(15) Uiso 0.560(12) 1 d PG A 2 
C304 C 0.1753(15) 0.1089(9) 0.7418(12) 0.31(2) Uiso 0.560(12) 1 d PG A 2 
Si1 Si 0.3389(3) 0.42267(18) -0.0573(2) 0.0172(9) Uani 1 1 d . . . 
Si2 Si 0.1935(3) 0.30634(19) -0.02881(18) 0.0196(9) Uani 1 1 d . . . 
Si3 Si -0.0280(3) 0.27964(18) -0.06228(19) 0.0175(9) Uani 1 1 d . . . 
Si4 Si -0.0249(3) 0.12212(17) -0.06371(18) 0.0155(9) Uani 1 1 d . . . 
Si5 Si 0.1862(3) 0.07164(18) -0.02853(17) 0.0152(9) Uani 1 1 d . . . 
Si6 Si 0.3329(3) 0.18426(19) -0.0588(2) 0.0202(9) Uani 1 1 d . . . 
Si7 Si 0.3266(3) 0.42320(18) 0.17192(18) 0.0180(9) Uani 1 1 d . . . 
Si8 Si 0.1887(3) 0.3065(2) 0.1288(2) 0.0205(9) Uani 1 1 d . . . 
Si9 Si -0.0279(3) 0.27451(19) 0.17274(18) 0.0175(9) Uani 1 1 d . . . 
Si10 Si -0.0260(3) 0.11987(18) 0.17348(18) 0.0191(9) Uani 1 1 d . . . 
Si11 Si 0.1860(3) 0.06957(19) 0.12963(19) 0.0183(9) Uani 1 1 d . . . 
Si12 Si 0.3223(3) 0.1857(2) 0.17256(19) 0.0185(9) Uani 1 1 d . . . 
Si13 Si 0.3400(3) 0.42273(18) 0.5578(2) 0.0168(9) Uani 1 1 d . . . 
Si14 Si 0.1938(3) 0.3069(2) 0.53009(18) 0.0197(9) Uani 1 1 d . . . 
Si15 Si -0.0276(3) 0.28037(18) 0.5613(2) 0.0194(9) Uani 1 1 d . . . 
Si16 Si -0.0245(3) 0.12334(18) 0.56393(19) 0.0182(9) Uani 1 1 d . . . 
Si17 Si 0.1884(3) 0.07096(18) 0.52854(18) 0.0155(9) Uani 1 1 d . . . 
Si18 Si 0.3319(3) 0.18484(18) 0.5599(2) 0.0184(9) Uani 1 1 d . . . 
Si19 Si 0.3284(3) 0.42214(18) 0.32785(18) 0.0175(9) Uani 1 1 d . . . 
Si20 Si 0.1879(3) 0.30667(19) 0.37068(19) 0.0163(8) Uani 1 1 d . . . 
Si21 Si -0.0280(3) 0.2747(2) 0.32821(19) 0.0192(9) Uani 1 1 d . . . 
Si22 Si -0.0253(3) 0.12001(18) 0.32710(18) 0.0186(9) Uani 1 1 d . . . 
Si23 Si 0.1852(3) 0.06976(18) 0.37023(19) 0.0153(8) Uani 1 1 d . . . 
Si24 Si 0.3222(3) 0.18541(19) 0.32689(18) 0.0173(9) Uani 1 1 d . . . 
O1 O 0.2522(7) 0.3714(5) -0.0519(6) 0.046(3) Uani 1 1 d . . . 
O2 O 0.0859(7) 0.3075(5) -0.0598(5) 0.036(3) Uani 1 1 d . . . 
O3 O -0.0319(9) 0.2004(4) -0.0606(6) 0.052(3) Uani 1 1 d . . . 
O4 O 0.0883(6) 0.0979(5) -0.0616(5) 0.033(3) Uani 1 1 d . . . 
O5 O 0.2792(6) 0.1146(4) -0.0561(5) 0.030(3) Uani 1 1 d . . . 
O6 O 0.2505(7) 0.2402(5) -0.0506(6) 0.048(3) Uani 1 1 d . . . 
O7 O 0.2410(8) 0.3714(5) 0.1547(5) 0.045(3) Uani 1 1 d . . . 
O8 O 0.0754(8) 0.3046(5) 0.1588(5) 0.041(3) Uani 1 1 d . . . 
O9 O -0.0194(9) 0.1959(5) 0.1553(4) 0.043(3) Uani 1 1 d . . . 
O10 O 0.0826(8) 0.0908(6) 0.1643(5) 0.044(3) Uani 1 1 d . . . 
O11 O 0.2791(7) 0.1145(5) 0.1565(5) 0.032(2) Uani 1 1 d . . . 
O12 O 0.2501(8) 0.2418(6) 0.1527(5) 0.050(3) Uani 1 1 d . . . 
O13 O 0.1960(9) 0.3069(6) 0.0490(6) 0.064(3) Uani 1 1 d . . . 
O14 O 0.1749(7) 0.0781(5) 0.0501(5) 0.039(3) Uani 1 1 d . . . 
O15 O 0.3997(7) 0.4186(5) -0.1279(5) 0.037(3) Uani 1 1 d . . . 
O16 O 0.4114(7) 0.4080(6) 0.0023(5) 0.042(3) Uani 1 1 d . . . 
O17 O 0.4267(7) 0.4014(6) 0.1333(5) 0.038(3) Uani 1 1 d . . . 
O18 O 0.3890(7) 0.1905(5) -0.1298(5) 0.034(3) Uani 1 1 d . . . 
O19 O 0.4158(8) 0.1904(5) -0.0022(5) 0.034(3) Uani 1 1 d . . . 
O20 O 0.4223(8) 0.1960(5) 0.1300(4) 0.033(3) Uani 1 1 d . . . 
O21 O 0.2037(7) -0.0047(4) -0.0513(5) 0.030(2) Uani 1 1 d . . . 
O22 O 0.2107(8) -0.0058(5) 0.1488(5) 0.035(3) Uani 1 1 d . . . 
O23 O 0.3526(3) 0.4234(2) 0.2510(6) 0.0398(11) Uani 1 1 d . . . 
O24 O 0.3514(3) 0.19042(18) 0.2505(6) 0.0316(9) Uani 1 1 d . . . 
O25 O -0.0512(3) 0.28397(19) 0.2480(6) 0.0310(10) Uani 1 1 d . . . 
O26 O -0.0581(3) 0.11092(17) 0.2486(6) 0.0262(9) Uani 1 1 d . . . 
O27 O 0.2489(7) 0.3696(5) 0.5597(5) 0.034(2) Uani 1 1 d . . . 
O28 O 0.0818(6) 0.3064(4) 0.5589(5) 0.032(2) Uani 1 1 d . . . 
O29 O -0.0285(8) 0.2014(4) 0.5570(6) 0.048(3) Uani 1 1 d . . . 
O30 O 0.0876(7) 0.0998(5) 0.5635(5) 0.036(3) Uani 1 1 d . . . 
O31 O 0.2812(6) 0.1119(4) 0.5535(5) 0.028(2) Uani 1 1 d . . . 
O32 O 0.2493(7) 0.2431(5) 0.5558(6) 0.038(3) Uani 1 1 d . . . 
O33 O 0.2396(7) 0.3706(5) 0.3395(5) 0.038(3) Uani 1 1 d . . . 
O34 O 0.0769(7) 0.3079(5) 0.3500(5) 0.036(3) Uani 1 1 d . . . 
O35 O -0.0299(8) 0.1975(4) 0.3483(4) 0.031(2) Uani 1 1 d . . . 
O36 O 0.0836(8) 0.0919(6) 0.3379(5) 0.048(3) Uani 1 1 d . . . 
O37 O 0.2684(7) 0.1154(5) 0.3405(5) 0.041(3) Uani 1 1 d . . . 
O38 O 0.2386(7) 0.2415(5) 0.3427(5) 0.044(3) Uani 1 1 d . . . 
O39 O 0.1850(9) 0.3083(6) 0.4484(5) 0.061(3) Uani 1 1 d . . . 
O40 O 0.1787(7) 0.0785(5) 0.4491(5) 0.038(3) Uani 1 1 d . . . 
O41 O 0.3924(8) 0.4185(5) 0.6264(5) 0.038(3) Uani 1 1 d . . . 
O42 O 0.4210(7) 0.4088(5) 0.4989(5) 0.033(2) Uani 1 1 d . . . 
O43 O 0.4261(7) 0.4007(5) 0.3684(4) 0.032(3) Uani 1 1 d . . . 
O44 O 0.3841(7) 0.1883(5) 0.6305(5) 0.030(3) Uani 1 1 d . . . 
O45 O 0.4098(8) 0.1925(5) 0.4995(5) 0.043(3) Uani 1 1 d . . . 
O46 O -0.0789(8) 0.3068(5) -0.1289(5) 0.045(3) Uani 1 1 d . . . 
O47 O 0.2070(6) -0.0038(4) 0.5474(4) 0.024(2) Uani 1 1 d . . . 
O48 O 0.2085(7) -0.0064(5) 0.3525(5) 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 
C101 C103 0.51(3) 3_657 ? 
C101 C102 0.90(4) 3_657 ? 
C101 C102 1.5054 . ? 
C101 C104 1.88(5) 3_657 ? 
C102 C101 0.90(4) 3_657 ? 
C102 C102 1.17(5) 3_657 ? 
C102 C103 1.3456 . ? 
C102 C103 1.78(5) 3_657 ? 
C103 C101 0.51(3) 3_657 ? 
C103 C104 1.5053 . ? 
C103 C102 1.78(4) 3_657 ? 
C104 C101 1.88(4) 3_657 ? 
C301 C302 1.5055 . ? 
C302 C303 1.3454 . ? 
C303 C304 1.5054 . ? 
Si1 O1 1.563(9) . ? 
Si1 O16 1.569(10) . ? 
Si1 O47 1.617(9) 2 ? 
Si1 O15 1.633(10) . ? 
Si2 O13 1.556(11) . ? 
Si2 O2 1.577(10) . ? 
Si2 O6 1.598(9) . ? 
Si2 O1 1.599(10) . ? 
Si3 O46 1.594(10) . ? 
Si3 O45 1.594(10) 4_565 ? 
Si3 O3 1.598(9) . ? 
Si3 O2 1.634(10) . ? 
Si4 O42 1.577(9) 4_565 ? 
Si4 O43 1.578(10) 4_565 ? 
Si4 O3 1.583(9) . ? 
Si4 O4 1.601(9) . ? 
Si5 O4 1.567(9) . ? 
Si5 O14 1.585(10) . ? 
Si5 O5 1.619(9) . ? 
Si5 O21 1.622(9) . ? 
Si6 O5 1.580(9) . ? 
Si6 O6 1.591(9) . ? 
Si6 O19 1.593(11) . ? 
Si6 O18 1.613(9) . ? 
Si7 O48 1.573(10) 2 ? 
Si7 O7 1.593(10) . ? 
Si7 O17 1.613(9) . ? 
Si7 O23 1.620(12) . ? 
Si8 O7 1.574(11) . ? 
Si8 O13 1.598(11) . ? 
Si8 O12 1.616(11) . ? 
Si8 O8 1.640(11) . ? 
Si9 O8 1.542(10) . ? 
Si9 O25 1.548(11) . ? 
Si9 O9 1.626(10) . ? 
Si9 O44 1.637(10) 4_565 ? 
Si10 O26 1.573(11) . ? 
Si10 O9 1.578(9) . ? 
Si10 O10 1.586(11) . ? 
Si10 O41 1.641(10) 4_565 ? 
Si11 O22 1.602(11) . ? 
Si11 O14 1.606(11) . ? 
Si11 O10 1.612(11) . ? 
Si11 O11 1.638(10) . ? 
Si12 O12 1.544(11) . ? 
Si12 O11 1.582(10) . ? 
Si12 O20 1.605(10) . ? 
Si12 O24 1.610(12) . ? 
Si13 O41 1.544(10) . ? 
Si13 O21 1.582(9) 2 ? 
Si13 O27 1.629(9) . ? 
Si13 O42 1.629(9) . ? 
Si14 O32 1.574(10) . ? 
Si14 O27 1.582(10) . ? 
Si14 O28 1.614(9) . ? 
Si14 O39 1.638(11) . ? 
Si15 O28 1.565(9) . ? 
Si15 O29 1.594(9) . ? 
Si15 O19 1.594(10) 4_566 ? 
Si15 O20 1.603(9) 4_566 ? 
Si16 O29 1.582(9) . ? 
Si16 O30 1.582(9) . ? 
Si16 O17 1.614(9) 4_566 ? 
Si16 O16 1.632(10) 4_566 ? 
Si17 O47 1.575(9) . ? 
Si17 O31 1.580(9) . ? 
Si17 O40 1.601(10) . ? 
Si17 O30 1.633(9) . ? 
Si18 O44 1.578(10) . ? 
Si18 O45 1.607(11) . ? 
Si18 O32 1.619(9) . ? 
Si18 O31 1.625(9) . ? 
Si19 O23 1.570(12) . ? 
Si19 O33 1.601(10) . ? 
Si19 O43 1.604(10) . ? 
Si19 O22 1.615(10) 2 ? 
Si20 O34 1.550(11) . ? 
Si20 O39 1.554(11) . ? 
Si20 O38 1.582(10) . ? 
Si20 O33 1.592(10) . ? 
Si21 O18 1.565(9) 4_566 ? 
Si21 O35 1.607(9) . ? 
Si21 O34 1.623(10) . ? 
Si21 O25 1.645(11) . ? 
Si22 O15 1.561(10) 4_566 ? 
Si22 O36 1.587(11) . ? 
Si22 O35 1.620(9) . ? 
Si22 O26 1.641(11) . ? 
Si23 O37 1.568(10) . ? 
Si23 O36 1.577(11) . ? 
Si23 O40 1.588(10) . ? 
Si23 O48 1.607(10) . ? 
Si24 O24 1.579(12) . ? 
Si24 O46 1.607(11) 4_666 ? 
Si24 O37 1.609(10) . ? 
Si24 O38 1.627(10) . ? 
O15 Si22 1.561(10) 4_665 ? 
O16 Si16 1.632(10) 4_665 ? 
O17 Si16 1.614(9) 4_665 ? 
O18 Si21 1.565(9) 4_665 ? 
O19 Si15 1.594(10) 4_665 ? 
O20 Si15 1.603(9) 4_665 ? 
O21 Si13 1.582(9) 2_545 ? 
O22 Si19 1.615(10) 2_545 ? 
O41 Si10 1.641(10) 4_666 ? 
O42 Si4 1.577(9) 4_666 ? 
O43 Si4 1.578(10) 4_666 ? 
O44 Si9 1.637(10) 4_666 ? 
O45 Si3 1.594(10) 4_666 ? 
O46 Si24 1.607(11) 4_565 ? 
O47 Si1 1.617(9) 2_545 ? 
O48 Si7 1.573(10) 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 C102 143(8) 3_657 3_657 ? 
C103 C101 C102 114(6) 3_657 . ? 
C102 C101 C102 51(3) 3_657 . ? 
C103 C101 C104 37(5) 3_657 3_657 ? 
C102 C101 C104 128(4) 3_657 3_657 ? 
C102 C101 C104 81(2) . 3_657 ? 
C101 C102 C102 92(4) 3_657 3_657 ? 
C101 C102 C103 13(2) 3_657 . ? 
C102 C102 C103 89.7(18) 3_657 . ? 
C101 C102 C101 129(3) 3_657 . ? 
C102 C102 C101 36.8(19) 3_657 . ? 
C103 C102 C101 125.4 . . ? 
C101 C102 C103 140(5) 3_657 3_657 ? 
C102 C102 C103 49.3(17) 3_657 3_657 ? 
C103 C102 C103 138.9(17) . 3_657 ? 
C101 C102 C103 15.2(15) . 3_657 ? 
C101 C103 C102 24(5) 3_657 . ? 
C101 C103 C104 131(5) 3_657 . ? 
C102 C103 C104 125.4 . . ? 
C101 C103 C102 51(4) 3_657 3_657 ? 
C102 C103 C102 41.1(14) . 3_657 ? 
C104 C103 C102 84.7(14) . 3_657 ? 
C103 C104 C101 11.9(13) . 3_657 ? 
C303 C302 C301 125.4 . . ? 
C302 C303 C304 125.4 . . ? 
O1 Si1 O16 106.8(6) . . ? 
O1 Si1 O47 108.2(5) . 2 ? 
O16 Si1 O47 108.5(6) . 2 ? 
O1 Si1 O15 113.6(6) . . ? 
O16 Si1 O15 109.6(6) . . ? 
O47 Si1 O15 110.0(5) 2 . ? 
O13 Si2 O2 114.4(6) . . ? 
O13 Si2 O6 105.5(7) . . ? 
O2 Si2 O6 110.3(6) . . ? 
O13 Si2 O1 105.8(7) . . ? 
O2 Si2 O1 109.1(6) . . ? 
O6 Si2 O1 111.6(6) . . ? 
O46 Si3 O45 107.5(6) . 4_565 ? 
O46 Si3 O3 110.3(6) . . ? 
O45 Si3 O3 108.6(6) 4_565 . ? 
O46 Si3 O2 108.1(6) . . ? 
O45 Si3 O2 110.3(6) 4_565 . ? 
O3 Si3 O2 112.0(6) . . ? 
O42 Si4 O43 112.0(6) 4_565 4_565 ? 
O42 Si4 O3 109.6(6) 4_565 . ? 
O43 Si4 O3 107.5(6) 4_565 . ? 
O42 Si4 O4 107.3(6) 4_565 . ? 
O43 Si4 O4 109.4(6) 4_565 . ? 
O3 Si4 O4 111.1(6) . . ? 
O4 Si5 O14 108.1(6) . . ? 
O4 Si5 O5 109.1(5) . . ? 
O14 Si5 O5 111.5(6) . . ? 
O4 Si5 O21 108.9(6) . . ? 
O14 Si5 O21 111.7(5) . . ? 
O5 Si5 O21 107.4(5) . . ? 
O5 Si6 O6 107.9(5) . . ? 
O5 Si6 O19 111.5(6) . . ? 
O6 Si6 O19 111.1(6) . . ? 
O5 Si6 O18 108.3(5) . . ? 
O6 Si6 O18 111.2(6) . . ? 
O19 Si6 O18 106.8(6) . . ? 
O48 Si7 O7 107.8(6) 2 . ? 
O48 Si7 O17 110.4(6) 2 . ? 
O7 Si7 O17 108.8(6) . . ? 
O48 Si7 O23 111.5(5) 2 . ? 
O7 Si7 O23 111.7(5) . . ? 
O17 Si7 O23 106.7(5) . . ? 
O7 Si8 O13 107.3(6) . . ? 
O7 Si8 O12 110.2(6) . . ? 
O13 Si8 O12 105.5(6) . . ? 
O7 Si8 O8 108.4(6) . . ? 
O13 Si8 O8 115.0(6) . . ? 
O12 Si8 O8 110.4(6) . . ? 
O8 Si9 O25 108.0(5) . . ? 
O8 Si9 O9 106.3(6) . . ? 
O25 Si9 O9 110.1(4) . . ? 
O8 Si9 O44 112.3(6) . 4_565 ? 
O25 Si9 O44 107.3(4) . 4_565 ? 
O9 Si9 O44 112.7(6) . 4_565 ? 
O26 Si10 O9 110.3(4) . . ? 
O26 Si10 O10 108.7(5) . . ? 
O9 Si10 O10 106.3(6) . . ? 
O26 Si10 O41 108.0(5) . 4_565 ? 
O9 Si10 O41 111.2(6) . 4_565 ? 
O10 Si10 O41 112.1(6) . 4_565 ? 
O22 Si11 O14 111.0(5) . . ? 
O22 Si11 O10 109.2(6) . . ? 
O14 Si11 O10 108.5(5) . . ? 
O22 Si11 O11 106.6(5) . . ? 
O14 Si11 O11 109.7(6) . . ? 
O10 Si11 O11 111.9(5) . . ? 
O12 Si12 O11 112.4(6) . . ? 
O12 Si12 O20 107.3(6) . . ? 
O11 Si12 O20 108.5(5) . . ? 
O12 Si12 O24 111.1(5) . . ? 
O11 Si12 O24 109.9(5) . . ? 
O20 Si12 O24 107.6(4) . . ? 
O41 Si13 O21 107.2(6) . 2 ? 
O41 Si13 O27 106.6(6) . . ? 
O21 Si13 O27 109.2(5) 2 . ? 
O41 Si13 O42 109.0(6) . . ? 
O21 Si13 O42 110.4(5) 2 . ? 
O27 Si13 O42 114.1(5) . . ? 
O32 Si14 O27 108.0(6) . . ? 
O32 Si14 O28 108.7(5) . . ? 
O27 Si14 O28 108.0(5) . . ? 
O32 Si14 O39 112.0(6) . . ? 
O27 Si14 O39 113.2(6) . . ? 
O28 Si14 O39 106.8(6) . . ? 
O28 Si15 O29 109.9(6) . . ? 
O28 Si15 O19 107.7(6) . 4_566 ? 
O29 Si15 O19 108.8(6) . 4_566 ? 
O28 Si15 O20 108.8(6) . 4_566 ? 
O29 Si15 O20 109.9(6) . 4_566 ? 
O19 Si15 O20 111.8(6) 4_566 4_566 ? 
O29 Si16 O30 109.3(6) . . ? 
O29 Si16 O17 111.7(6) . 4_566 ? 
O30 Si16 O17 107.5(6) . 4_566 ? 
O29 Si16 O16 107.5(6) . 4_566 ? 
O30 Si16 O16 112.6(6) . 4_566 ? 
O17 Si16 O16 108.3(6) 4_566 4_566 ? 
O47 Si17 O31 107.4(5) . . ? 
O47 Si17 O40 110.0(5) . . ? 
O31 Si17 O40 109.2(6) . . ? 
O47 Si17 O30 111.7(5) . . ? 
O31 Si17 O30 109.7(5) . . ? 
O40 Si17 O30 108.8(5) . . ? 
O44 Si18 O45 112.1(6) . . ? 
O44 Si18 O32 108.6(6) . . ? 
O45 Si18 O32 110.0(6) . . ? 
O44 Si18 O31 107.3(5) . . ? 
O45 Si18 O31 107.5(6) . . ? 
O32 Si18 O31 111.3(5) . . ? 
O23 Si19 O33 107.9(5) . . ? 
O23 Si19 O43 109.2(4) . . ? 
O33 Si19 O43 111.3(5) . . ? 
O23 Si19 O22 109.7(4) . 2 ? 
O33 Si19 O22 107.4(6) . 2 ? 
O43 Si19 O22 111.3(6) . 2 ? 
O34 Si20 O39 104.0(6) . . ? 
O34 Si20 O38 109.6(6) . . ? 
O39 Si20 O38 112.4(6) . . ? 
O34 Si20 O33 107.7(6) . . ? 
O39 Si20 O33 112.6(6) . . ? 
O38 Si20 O33 110.2(6) . . ? 
O18 Si21 O35 106.8(6) 4_566 . ? 
O18 Si21 O34 107.0(5) 4_566 . ? 
O35 Si21 O34 110.3(6) . . ? 
O18 Si21 O25 109.7(5) 4_566 . ? 
O35 Si21 O25 110.5(4) . . ? 
O34 Si21 O25 112.4(5) . . ? 
O15 Si22 O36 109.9(6) 4_566 . ? 
O15 Si22 O35 107.8(5) 4_566 . ? 
O36 Si22 O35 110.2(6) . . ? 
O15 Si22 O26 108.8(5) 4_566 . ? 
O36 Si22 O26 109.8(5) . . ? 
O35 Si22 O26 110.3(4) . . ? 
O37 Si23 O36 107.4(6) . . ? 
O37 Si23 O40 110.5(6) . . ? 
O36 Si23 O40 109.1(6) . . ? 
O37 Si23 O48 109.8(5) . . ? 
O36 Si23 O48 110.4(6) . . ? 
O40 Si23 O48 109.6(5) . . ? 
O24 Si24 O46 108.6(4) . 4_666 ? 
O24 Si24 O37 109.4(5) . . ? 
O46 Si24 O37 111.5(6) 4_666 . ? 
O24 Si24 O38 108.4(5) . . ? 
O46 Si24 O38 113.5(6) 4_666 . ? 
O37 Si24 O38 105.3(5) . . ? 
Si1 O1 Si2 158.6(8) . . ? 
Si2 O2 Si3 150.4(7) . . ? 
Si4 O3 Si3 173.7(9) . . ? 
Si5 O4 Si4 156.2(8) . . ? 
Si6 O5 Si5 147.2(6) . . ? 
Si6 O6 Si2 162.6(8) . . ? 
Si8 O7 Si7 160.1(8) . . ? 
Si9 O8 Si8 156.1(8) . . ? 
Si10 O9 Si9 153.2(6) . . ? 
Si10 O10 Si11 160.6(7) . . ? 
Si12 O11 Si11 148.2(7) . . ? 
Si12 O12 Si8 171.7(8) . . ? 
Si2 O13 Si8 175.2(9) . . ? 
Si5 O14 Si11 164.6(7) . . ? 
Si22 O15 Si1 147.9(8) 4_665 . ? 
Si1 O16 Si16 167.4(9) . 4_665 ? 
Si7 O17 Si16 146.6(7) . 4_665 ? 
Si21 O18 Si6 147.4(7) 4_665 . ? 
Si6 O19 Si15 158.3(8) . 4_665 ? 
Si15 O20 Si12 147.7(7) 4_665 . ? 
Si13 O21 Si5 147.8(6) 2_545 . ? 
Si11 O22 Si19 148.7(7) . 2_545 ? 
Si19 O23 Si7 155.5(3) . . ? 
Si24 O24 Si12 150.6(2) . . ? 
Si9 O25 Si21 153.5(3) . . ? 
Si10 O26 Si22 145.7(2) . . ? 
Si14 O27 Si13 150.5(7) . . ? 
Si15 O28 Si14 153.2(7) . . ? 
Si16 O29 Si15 171.5(8) . . ? 
Si16 O30 Si17 154.4(7) . . ? 
Si17 O31 Si18 146.1(7) . . ? 
Si14 O32 Si18 159.2(7) . . ? 
Si20 O33 Si19 155.4(8) . . ? 
Si20 O34 Si21 154.7(7) . . ? 
Si21 O35 Si22 150.3(6) . . ? 
Si23 O36 Si22 163.4(8) . . ? 
Si23 O37 Si24 154.3(7) . . ? 
Si20 O38 Si24 160.8(8) . . ? 
Si20 O39 Si14 174.0(8) . . ? 
Si23 O40 Si17 165.8(7) . . ? 
Si13 O41 Si10 147.3(7) . 4_666 ? 
Si4 O42 Si13 162.0(7) 4_666 . ? 
Si4 O43 Si19 148.9(7) 4_666 . ? 
Si18 O44 Si9 143.5(6) . 4_666 ? 
Si3 O45 Si18 163.4(8) 4_666 . ? 
Si3 O46 Si24 148.1(7) . 4_565 ? 
Si17 O47 Si1 147.8(6) . 2_545 ? 
Si7 O48 Si23 150.7(7) 2_545 . ? 
  
_diffrn_measured_fraction_theta_max    0.932 
_diffrn_reflns_theta_full              28.66 
_diffrn_measured_fraction_theta_full   0.932 
_refine_diff_density_max    0.882 
_refine_diff_density_min   -0.488 
_refine_diff_density_rms    0.129 





  
data_f_ip_twin_02 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C1.3 H0 O48 Si24' 
_chemical_formula_weight          1458 
  
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                    13.29(2) 
_cell_length_b                    20.02(3) 
_cell_length_c                    19.79(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.04(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      5265(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           0.17 
_exptl_crystal_size_mid           0.12 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.910 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3048 
_exptl_absorpt_coefficient_mu     0.689 
_exptl_absorpt_correction_type    Analytical 
_exptl_absorpt_correction_T_min   0.8902 
_exptl_absorpt_correction_T_max   0.9534 
_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             61824 
_diffrn_reflns_av_R_equivalents   0.1062 
_diffrn_reflns_av_sigmaI/netI     0.1134 
_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          1.02 
_diffrn_reflns_theta_max          28.75 
_reflns_number_total              12864 
_reflns_number_gt                 6589 
_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)+(0.0468P)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          12864 
_refine_ls_number_parameters      671 
_refine_ls_number_restraints      8 
_refine_ls_R_factor_all           0.1203 
_refine_ls_R_factor_gt            0.0549 
_refine_ls_wR_factor_ref          0.1273 
_refine_ls_wR_factor_gt           0.1102 
_refine_ls_goodness_of_fit_ref    0.872 
_refine_ls_restrained_S_all       0.889 
_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 0.109(10) 0.403(4) 0.729(8) 0.65(11) Uiso 0.261(16) 1 d PD A 1 
C103 C 0.138(8) 0.508(6) 0.797(4) 0.38(8) Uiso 0.261(16) 1 d PD A 1 
C102 C 0.059(7) 0.459(4) 0.770(5) 1.0(2) Uiso 0.261(16) 1 d PD A 1 
C105 C 0.005(6) 0.506(4) 0.705(4) 0.29(5) Uiso 0.261(16) 1 d PD A 1 
C104 C 0.233(9) 0.541(5) 0.768(8) 0.45(8) Uiso 0.261(16) 1 d PD A 1 
Si1 Si 0.32303(15) 0.42071(8) -0.05575(11) 0.0160(4) Uani 1 1 d . . . 
Si2 Si 0.16811(15) 0.31270(10) -0.03011(9) 0.0180(4) Uani 1 1 d . . . 
Si3 Si -0.04878(15) 0.27942(9) -0.06248(10) 0.0175(4) Uani 1 1 d . . . 
Si4 Si -0.03493(14) 0.12366(9) -0.06284(10) 0.0159(4) Uani 1 1 d . . . 
Si5 Si 0.17752(16) 0.07602(9) -0.02816(9) 0.0145(4) Uani 1 1 d . . . 
Si6 Si 0.31589(15) 0.19411(9) -0.05603(11) 0.0181(4) Uani 1 1 d . . . 
Si7 Si 0.31986(16) 0.42509(9) 0.17159(10) 0.0164(4) Uani 1 1 d . . . 
Si8 Si 0.17577(15) 0.31120(10) 0.12723(9) 0.0172(4) Uani 1 1 d . . . 
Si9 Si -0.03584(15) 0.27308(9) 0.17554(10) 0.0172(4) Uani 1 1 d . . . 
Si10 Si -0.03297(16) 0.11899(9) 0.17548(9) 0.0177(5) Uani 1 1 d . . . 
Si11 Si 0.17754(16) 0.07116(9) 0.12922(10) 0.0172(4) Uani 1 1 d . . . 
Si12 Si 0.31509(16) 0.19004(10) 0.16664(9) 0.0173(4) Uani 1 1 d . . . 
Si13 Si 0.33498(14) 0.42769(8) 0.55713(11) 0.0154(4) Uani 1 1 d . . . 
Si14 Si 0.18870(15) 0.31179(10) 0.52741(9) 0.0181(4) Uani 1 1 d . . . 
Si15 Si -0.02972(14) 0.27773(9) 0.56125(10) 0.0162(4) Uani 1 1 d . . . 
Si16 Si -0.03258(14) 0.12172(9) 0.56428(10) 0.0163(4) Uani 1 1 d . . . 
Si17 Si 0.18018(16) 0.07067(9) 0.52745(9) 0.0147(4) Uani 1 1 d . . . 
Si18 Si 0.31892(15) 0.18715(9) 0.56223(10) 0.0165(4) Uani 1 1 d . . . 
Si19 Si 0.31606(16) 0.42385(9) 0.32795(9) 0.0160(4) Uani 1 1 d . . . 
Si20 Si 0.17160(15) 0.31200(9) 0.36921(10) 0.0179(4) Uani 1 1 d . . . 
Si21 Si -0.04309(15) 0.27315(9) 0.33081(9) 0.0175(5) Uani 1 1 d . . . 
Si22 Si -0.03656(16) 0.11862(10) 0.32931(10) 0.0174(4) Uani 1 1 d . . . 
Si23 Si 0.17800(16) 0.07208(8) 0.36953(10) 0.0158(4) Uani 1 1 d . . . 
Si24 Si 0.30162(15) 0.19303(9) 0.32062(9) 0.0174(4) Uani 1 1 d . . . 
O1 O 0.2252(4) 0.3768(2) -0.0578(3) 0.0359(13) Uani 1 1 d . . . 
O2 O 0.0605(3) 0.3105(2) -0.0650(2) 0.0275(12) Uani 1 1 d . . . 
O3 O -0.0439(4) 0.2017(2) -0.0505(3) 0.0427(13) Uani 1 1 d . . . 
O4 O 0.0792(3) 0.1030(2) -0.0668(2) 0.0284(12) Uani 1 1 d . . . 
O5 O 0.2718(3) 0.1208(2) -0.0467(3) 0.0259(12) Uani 1 1 d . . . 
O6 O 0.2287(4) 0.2467(2) -0.0470(3) 0.0408(14) Uani 1 1 d . . . 
O7 O 0.2295(4) 0.3760(3) 0.1547(3) 0.0396(16) Uani 1 1 d . . . 
O8 O 0.0702(4) 0.3050(2) 0.1654(2) 0.0353(13) Uani 1 1 d . . . 
O9 O -0.0312(4) 0.1955(2) 0.1560(2) 0.0307(13) Uani 1 1 d . . . 
O10 O 0.0768(4) 0.0890(3) 0.1683(2) 0.0349(14) Uani 1 1 d . . . 
O11 O 0.2663(4) 0.1201(3) 0.1514(3) 0.0367(15) Uani 1 1 d . . . 
O12 O 0.2420(4) 0.2477(3) 0.1395(2) 0.0431(15) Uani 1 1 d . . . 
O13 O 0.1557(4) 0.3181(3) 0.0496(3) 0.0468(15) Uani 1 1 d . . . 
O14 O 0.1570(3) 0.0783(2) 0.0507(2) 0.0282(11) Uani 1 1 d . . . 
O15 O 0.3783(4) 0.4143(3) -0.1254(2) 0.0390(15) Uani 1 1 d . . . 
O16 O 0.3943(4) 0.3959(3) 0.0042(2) 0.0441(16) Uani 1 1 d . . . 
O17 O 0.4191(4) 0.4006(2) 0.1342(2) 0.0256(12) Uani 1 1 d . . . 
O18 O 0.3616(3) 0.2002(2) -0.1298(2) 0.0286(12) Uani 1 1 d . . . 
O19 O 0.4031(4) 0.2071(3) -0.0023(2) 0.0348(14) Uani 1 1 d . . . 
O20 O 0.4197(3) 0.1954(2) 0.1285(2) 0.0303(12) Uani 1 1 d . . . 
O21 O 0.2038(3) 0.00265(19) -0.0515(2) 0.0223(11) Uani 1 1 d . . . 
O22 O 0.2101(4) -0.0029(2) 0.1471(2) 0.0285(13) Uani 1 1 d . . . 
O23 O 0.3435(3) 0.42419(19) 0.2506(3) 0.0304(10) Uani 1 1 d . . . 
O24 O 0.3387(3) 0.19743(19) 0.2446(2) 0.0278(10) Uani 1 1 d . . . 
O25 O -0.0662(3) 0.28213(17) 0.2531(3) 0.0246(9) Uani 1 1 d . . . 
O26 O -0.0680(3) 0.10969(17) 0.2520(3) 0.0234(9) Uani 1 1 d . . . 
O27 O 0.2421(4) 0.3777(2) 0.5518(3) 0.0404(14) Uani 1 1 d . . . 
O28 O 0.0748(3) 0.3137(2) 0.5535(3) 0.0296(12) Uani 1 1 d . . . 
O29 O -0.0112(4) 0.1996(2) 0.5658(3) 0.0423(14) Uani 1 1 d . . . 
O30 O 0.0691(3) 0.0837(2) 0.5548(3) 0.0361(13) Uani 1 1 d . . . 
O31 O 0.2568(4) 0.1195(2) 0.5644(2) 0.0309(13) Uani 1 1 d . . . 
O32 O 0.2446(4) 0.2492(2) 0.5591(3) 0.0359(13) Uani 1 1 d . . . 
O33 O 0.2207(4) 0.3786(2) 0.3416(3) 0.0319(14) Uani 1 1 d . . . 
O34 O 0.0552(4) 0.3142(2) 0.3537(2) 0.0269(12) Uani 1 1 d . . . 
O35 O -0.0257(4) 0.1959(2) 0.3475(2) 0.0313(13) Uani 1 1 d . . . 
O36 O 0.0674(4) 0.0839(3) 0.3433(3) 0.0426(15) Uani 1 1 d . . . 
O37 O 0.2543(4) 0.1219(3) 0.3342(2) 0.0374(15) Uani 1 1 d . . . 
O38 O 0.2206(4) 0.2481(2) 0.3327(2) 0.0380(14) Uani 1 1 d . . . 
O39 O 0.1923(4) 0.3060(3) 0.4482(2) 0.0475(14) Uani 1 1 d . . . 
O40 O 0.1826(4) 0.0842(2) 0.4484(3) 0.0374(13) Uani 1 1 d . . . 
O41 O 0.3887(4) 0.4192(2) 0.6285(3) 0.0321(13) Uani 1 1 d . . . 
O42 O 0.4129(4) 0.4137(2) 0.4986(2) 0.0320(13) Uani 1 1 d . . . 
O43 O 0.4111(4) 0.3953(2) 0.3681(2) 0.0303(13) Uani 1 1 d . . . 
O44 O 0.3840(4) 0.1903(2) 0.6294(2) 0.0271(12) Uani 1 1 d . . . 
O45 O 0.3897(4) 0.1870(3) 0.4977(3) 0.0371(14) Uani 1 1 d . . . 
O46 O -0.1031(4) 0.2946(3) -0.1316(3) 0.0417(15) Uani 1 1 d . . . 
O47 O 0.2094(4) -0.0047(2) 0.5438(2) 0.0251(12) Uani 1 1 d . . . 
O48 O 0.2116(4) -0.0016(2) 0.3524(2) 0.0296(13) 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 1.53(2) . ? 
C103 C102 1.53(2) . ? 
C103 C104 1.53(2) . ? 
C102 C105 1.732(19) . ? 
Si1 O15 1.568(5) . ? 
Si1 O1 1.569(5) . ? 
Si1 O47 1.571(5) 2 ? 
Si1 O16 1.597(5) . ? 
Si2 O6 1.583(5) . ? 
Si2 O2 1.589(5) . ? 
Si2 O1 1.589(5) . ? 
Si2 O13 1.590(6) . ? 
Si3 O46 1.575(5) . ? 
Si3 O3 1.575(5) . ? 
Si3 O2 1.581(5) . ? 
Si3 O45 1.593(5) 4_565 ? 
Si4 O4 1.575(5) . ? 
Si4 O3 1.586(5) . ? 
Si4 O42 1.588(5) 4_565 ? 
Si4 O43 1.589(5) 4_565 ? 
Si5 O21 1.579(5) . ? 
Si5 O5 1.584(5) . ? 
Si5 O14 1.586(5) . ? 
Si5 O4 1.607(5) . ? 
Si6 O6 1.576(5) . ? 
Si6 O18 1.587(5) . ? 
Si6 O5 1.591(5) . ? 
Si6 O19 1.593(5) . ? 
Si7 O7 1.588(5) . ? 
Si7 O17 1.591(5) . ? 
Si7 O23 1.595(6) . ? 
Si7 O48 1.598(5) 2 ? 
Si8 O13 1.565(6) . ? 
Si8 O12 1.565(5) . ? 
Si8 O7 1.577(5) . ? 
Si8 O8 1.599(5) . ? 
Si9 O8 1.560(5) . ? 
Si9 O44 1.582(5) 4_565 ? 
Si9 O25 1.598(5) . ? 
Si9 O9 1.601(5) . ? 
Si10 O9 1.580(5) . ? 
Si10 O10 1.584(6) . ? 
Si10 O41 1.590(5) 4_565 ? 
Si10 O26 1.596(6) . ? 
Si11 O14 1.583(5) . ? 
Si11 O22 1.584(5) . ? 
Si11 O10 1.588(5) . ? 
Si11 O11 1.595(5) . ? 
Si12 O11 1.573(5) . ? 
Si12 O24 1.582(5) . ? 
Si12 O20 1.586(5) . ? 
Si12 O12 1.601(5) . ? 
Si13 O42 1.579(5) . ? 
Si13 O21 1.591(5) 2 ? 
Si13 O41 1.591(5) . ? 
Si13 O27 1.592(5) . ? 
Si14 O39 1.572(6) . ? 
Si14 O27 1.575(5) . ? 
Si14 O32 1.587(5) . ? 
Si14 O28 1.600(5) . ? 
Si15 O19 1.572(5) 4_566 ? 
Si15 O28 1.572(5) . ? 
Si15 O29 1.586(5) . ? 
Si15 O20 1.586(5) 4_566 ? 
Si16 O30 1.563(5) . ? 
Si16 O16 1.575(5) 4_566 ? 
Si16 O29 1.585(5) . ? 
Si16 O17 1.590(5) 4_566 ? 
Si17 O31 1.589(5) . ? 
Si17 O40 1.589(6) . ? 
Si17 O47 1.592(5) . ? 
Si17 O30 1.594(5) . ? 
Si18 O44 1.587(5) . ? 
Si18 O31 1.587(5) . ? 
Si18 O45 1.587(5) . ? 
Si18 O32 1.588(5) . ? 
Si19 O23 1.574(6) . ? 
Si19 O33 1.581(5) . ? 
Si19 O22 1.586(5) 2 ? 
Si19 O43 1.598(5) . ? 
Si20 O34 1.577(6) . ? 
Si20 O33 1.582(5) . ? 
Si20 O39 1.592(6) . ? 
Si20 O38 1.607(5) . ? 
Si21 O25 1.578(5) . ? 
Si21 O18 1.580(5) 4_566 ? 
Si21 O35 1.599(5) . ? 
Si21 O34 1.608(5) . ? 
Si22 O36 1.571(6) . ? 
Si22 O15 1.588(5) 4_566 ? 
Si22 O35 1.595(5) . ? 
Si22 O26 1.595(6) . ? 
Si23 O36 1.576(6) . ? 
Si23 O48 1.578(5) . ? 
Si23 O40 1.580(6) . ? 
Si23 O37 1.586(5) . ? 
Si24 O38 1.560(5) . ? 
Si24 O37 1.579(6) . ? 
Si24 O24 1.585(5) . ? 
Si24 O46 1.600(5) 4_666 ? 
O15 Si22 1.588(5) 4_665 ? 
O16 Si16 1.575(5) 4_665 ? 
O17 Si16 1.590(5) 4_665 ? 
O18 Si21 1.580(5) 4_665 ? 
O19 Si15 1.572(5) 4_665 ? 
O20 Si15 1.586(5) 4_665 ? 
O21 Si13 1.591(5) 2_545 ? 
O22 Si19 1.586(5) 2_545 ? 
O41 Si10 1.590(5) 4_666 ? 
O42 Si4 1.588(5) 4_666 ? 
O43 Si4 1.589(5) 4_666 ? 
O44 Si9 1.582(5) 4_666 ? 
O45 Si3 1.593(5) 4_666 ? 
O46 Si24 1.600(5) 4_565 ? 
O47 Si1 1.571(5) 2_545 ? 
O48 Si7 1.598(5) 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 
C102 C103 C104 135(9) . . ? 
C103 C102 C101 111(3) . . ? 
C103 C102 C105 101(3) . . ? 
C101 C102 C105 101(3) . . ? 
O15 Si1 O1 108.7(3) . . ? 
O15 Si1 O47 109.8(3) . 2 ? 
O1 Si1 O47 108.0(3) . 2 ? 
O15 Si1 O16 110.5(3) . . ? 
O1 Si1 O16 109.6(3) . . ? 
O47 Si1 O16 110.2(3) 2 . ? 
O6 Si2 O2 110.0(3) . . ? 
O6 Si2 O1 111.0(3) . . ? 
O2 Si2 O1 107.6(3) . . ? 
O6 Si2 O13 108.6(3) . . ? 
O2 Si2 O13 109.9(3) . . ? 
O1 Si2 O13 109.7(3) . . ? 
O46 Si3 O3 109.9(3) . . ? 
O46 Si3 O2 108.5(3) . . ? 
O3 Si3 O2 110.8(3) . . ? 
O46 Si3 O45 109.4(3) . 4_565 ? 
O3 Si3 O45 109.0(3) . 4_565 ? 
O2 Si3 O45 109.2(3) . 4_565 ? 
O4 Si4 O3 109.8(3) . . ? 
O4 Si4 O42 109.6(3) . 4_565 ? 
O3 Si4 O42 108.3(3) . 4_565 ? 
O4 Si4 O43 109.2(3) . 4_565 ? 
O3 Si4 O43 109.5(3) . 4_565 ? 
O42 Si4 O43 110.5(3) 4_565 4_565 ? 
O21 Si5 O5 106.5(3) . . ? 
O21 Si5 O14 110.7(3) . . ? 
O5 Si5 O14 110.3(3) . . ? 
O21 Si5 O4 110.7(3) . . ? 
O5 Si5 O4 110.0(3) . . ? 
O14 Si5 O4 108.6(3) . . ? 
O6 Si6 O18 109.5(3) . . ? 
O6 Si6 O5 109.4(3) . . ? 
O18 Si6 O5 108.6(3) . . ? 
O6 Si6 O19 110.5(3) . . ? 
O18 Si6 O19 108.8(3) . . ? 
O5 Si6 O19 109.9(3) . . ? 
O7 Si7 O17 109.8(3) . . ? 
O7 Si7 O23 110.3(3) . . ? 
O17 Si7 O23 106.8(3) . . ? 
O7 Si7 O48 108.0(3) . 2 ? 
O17 Si7 O48 111.2(3) . 2 ? 
O23 Si7 O48 110.7(3) . 2 ? 
O13 Si8 O12 108.6(3) . . ? 
O13 Si8 O7 110.1(3) . . ? 
O12 Si8 O7 111.1(3) . . ? 
O13 Si8 O8 108.8(3) . . ? 
O12 Si8 O8 110.9(3) . . ? 
O7 Si8 O8 107.3(3) . . ? 
O8 Si9 O44 110.1(3) . 4_565 ? 
O8 Si9 O25 107.8(3) . . ? 
O44 Si9 O25 109.4(3) 4_565 . ? 
O8 Si9 O9 109.3(3) . . ? 
O44 Si9 O9 109.6(3) 4_565 . ? 
O25 Si9 O9 110.6(2) . . ? 
O9 Si10 O10 109.4(3) . . ? 
O9 Si10 O41 109.4(3) . 4_565 ? 
O10 Si10 O41 111.6(3) . 4_565 ? 
O9 Si10 O26 110.4(2) . . ? 
O10 Si10 O26 108.0(3) . . ? 
O41 Si10 O26 107.9(3) 4_565 . ? 
O14 Si11 O22 110.5(3) . . ? 
O14 Si11 O10 108.2(3) . . ? 
O22 Si11 O10 109.4(3) . . ? 
O14 Si11 O11 110.0(3) . . ? 
O22 Si11 O11 108.2(3) . . ? 
O10 Si11 O11 110.6(3) . . ? 
O11 Si12 O24 110.6(3) . . ? 
O11 Si12 O20 109.3(3) . . ? 
O24 Si12 O20 106.5(3) . . ? 
O11 Si12 O12 109.2(3) . . ? 
O24 Si12 O12 112.3(3) . . ? 
O20 Si12 O12 108.9(3) . . ? 
O42 Si13 O21 109.2(3) . 2 ? 
O42 Si13 O41 109.7(3) . . ? 
O21 Si13 O41 108.0(3) 2 . ? 
O42 Si13 O27 110.5(3) . . ? 
O21 Si13 O27 109.7(3) 2 . ? 
O41 Si13 O27 109.8(3) . . ? 
O39 Si14 O27 110.8(3) . . ? 
O39 Si14 O32 108.7(3) . . ? 
O27 Si14 O32 109.3(3) . . ? 
O39 Si14 O28 110.6(3) . . ? 
O27 Si14 O28 107.9(3) . . ? 
O32 Si14 O28 109.5(3) . . ? 
O19 Si15 O28 109.6(3) 4_566 . ? 
O19 Si15 O29 108.9(3) 4_566 . ? 
O28 Si15 O29 108.7(3) . . ? 
O19 Si15 O20 111.4(3) 4_566 4_566 ? 
O28 Si15 O20 107.6(3) . 4_566 ? 
O29 Si15 O20 110.7(3) . 4_566 ? 
O30 Si16 O16 109.5(3) . 4_566 ? 
O30 Si16 O29 109.1(3) . . ? 
O16 Si16 O29 110.2(3) 4_566 . ? 
O30 Si16 O17 108.5(3) . 4_566 ? 
O16 Si16 O17 110.2(3) 4_566 4_566 ? 
O29 Si16 O17 109.4(3) . 4_566 ? 
O31 Si17 O40 109.5(3) . . ? 
O31 Si17 O47 109.5(3) . . ? 
O40 Si17 O47 110.9(3) . . ? 
O31 Si17 O30 109.6(3) . . ? 
O40 Si17 O30 109.1(3) . . ? 
O47 Si17 O30 108.2(3) . . ? 
O44 Si18 O31 107.2(3) . . ? 
O44 Si18 O45 110.5(3) . . ? 
O31 Si18 O45 109.2(3) . . ? 
O44 Si18 O32 109.9(3) . . ? 
O31 Si18 O32 110.2(3) . . ? 
O45 Si18 O32 109.9(3) . . ? 
O23 Si19 O33 110.8(3) . . ? 
O23 Si19 O22 110.5(3) . 2 ? 
O33 Si19 O22 107.5(3) . 2 ? 
O23 Si19 O43 107.6(3) . . ? 
O33 Si19 O43 110.1(3) . . ? 
O22 Si19 O43 110.4(3) 2 . ? 
O34 Si20 O33 108.3(3) . . ? 
O34 Si20 O39 111.2(3) . . ? 
O33 Si20 O39 109.4(3) . . ? 
O34 Si20 O38 109.4(3) . . ? 
O33 Si20 O38 110.4(3) . . ? 
O39 Si20 O38 108.2(3) . . ? 
O25 Si21 O18 106.6(3) . 4_566 ? 
O25 Si21 O35 109.8(2) . . ? 
O18 Si21 O35 109.9(3) 4_566 . ? 
O25 Si21 O34 112.0(2) . . ? 
O18 Si21 O34 109.9(3) 4_566 . ? 
O35 Si21 O34 108.6(3) . . ? 
O36 Si22 O15 110.1(3) . 4_566 ? 
O36 Si22 O35 108.0(3) . . ? 
O15 Si22 O35 109.9(3) 4_566 . ? 
O36 Si22 O26 110.4(3) . . ? 
O15 Si22 O26 108.0(3) 4_566 . ? 
O35 Si22 O26 110.4(2) . . ? 
O36 Si23 O48 109.5(3) . . ? 
O36 Si23 O40 109.7(3) . . ? 
O48 Si23 O40 110.2(3) . . ? 
O36 Si23 O37 110.9(3) . . ? 
O48 Si23 O37 108.2(3) . . ? 
O40 Si23 O37 108.3(3) . . ? 
O38 Si24 O37 109.7(3) . . ? 
O38 Si24 O24 108.7(3) . . ? 
O37 Si24 O24 109.6(2) . . ? 
O38 Si24 O46 110.3(3) . 4_666 ? 
O37 Si24 O46 110.7(3) . 4_666 ? 
O24 Si24 O46 107.8(3) . 4_666 ? 
Si1 O1 Si2 147.0(4) . . ? 
Si3 O2 Si2 145.5(3) . . ? 
Si3 O3 Si4 162.4(4) . . ? 
Si4 O4 Si5 147.9(3) . . ? 
Si5 O5 Si6 147.2(3) . . ? 
Si6 O6 Si2 162.8(4) . . ? 
Si8 O7 Si7 157.5(4) . . ? 
Si9 O8 Si8 152.3(4) . . ? 
Si10 O9 Si9 151.7(3) . . ? 
Si10 O10 Si11 154.9(4) . . ? 
Si12 O11 Si11 154.8(4) . . ? 
Si8 O12 Si12 168.2(4) . . ? 
Si8 O13 Si2 161.9(4) . . ? 
Si11 O14 Si5 159.0(3) . . ? 
Si1 O15 Si22 149.9(4) . 4_665 ? 
Si16 O16 Si1 174.8(4) 4_665 . ? 
Si16 O17 Si7 145.8(4) 4_665 . ? 
Si21 O18 Si6 141.9(3) 4_665 . ? 
Si15 O19 Si6 168.0(4) 4_665 . ? 
Si15 O20 Si12 142.6(3) 4_665 . ? 
Si5 O21 Si13 145.8(3) . 2_545 ? 
Si11 O22 Si19 151.0(4) . 2_545 ? 
Si19 O23 Si7 155.3(3) . . ? 
Si12 O24 Si24 149.2(3) . . ? 
Si21 O25 Si9 150.9(3) . . ? 
Si22 O26 Si10 145.2(3) . . ? 
Si14 O27 Si13 153.6(4) . . ? 
Si15 O28 Si14 149.0(3) . . ? 
Si16 O29 Si15 160.3(4) . . ? 
Si16 O30 Si17 157.2(4) . . ? 
Si18 O31 Si17 147.8(3) . . ? 
Si14 O32 Si18 157.6(4) . . ? 
Si19 O33 Si20 150.7(4) . . ? 
Si20 O34 Si21 146.8(3) . . ? 
Si22 O35 Si21 151.5(3) . . ? 
Si22 O36 Si23 160.8(4) . . ? 
Si24 O37 Si23 153.7(4) . . ? 
Si24 O38 Si20 155.7(4) . . ? 
Si14 O39 Si20 165.5(4) . . ? 
Si23 O40 Si17 161.0(3) . . ? 
Si10 O41 Si13 149.7(3) 4_666 . ? 
Si13 O42 Si4 158.7(4) . 4_666 ? 
Si4 O43 Si19 150.4(4) 4_666 . ? 
Si9 O44 Si18 150.3(3) 4_666 . ? 
Si18 O45 Si3 154.8(4) . 4_666 ? 
Si3 O46 Si24 154.9(4) . 4_565 ? 
Si1 O47 Si17 149.8(4) 2_545 . ? 
Si23 O48 Si7 148.0(4) . 2_545 ? 
  
_diffrn_measured_fraction_theta_max    0.942 
_diffrn_reflns_theta_full              28.75 
_diffrn_measured_fraction_theta_full   0.942 
_refine_diff_density_max    0.549 
_refine_diff_density_min   -0.599 
_refine_diff_density_rms    0.124 





  
data_f_butane_twin_3h 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C3.6 O48 Si24' 
_chemical_formula_weight          1485 
  
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                    13.462(6) 
_cell_length_b                    20.198(8) 
_cell_length_c                    19.990(9) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.091(12) 
_cell_angle_gamma                 90.00 
_cell_volume                      5435(4) 
_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           0.09 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.833 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3016 
_exptl_absorpt_coefficient_mu     0.666 
_exptl_absorpt_correction_type    Analytical 
_exptl_absorpt_correction_T_min   0.8963 
_exptl_absorpt_correction_T_max   0.9574 
_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             63654 
_diffrn_reflns_av_R_equivalents   0.1482 
_diffrn_reflns_av_sigmaI/netI     0.1636 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        27 
_diffrn_reflns_limit_l_min        -27 
_diffrn_reflns_limit_l_max        27 
_diffrn_reflns_theta_min          1.51 
_diffrn_reflns_theta_max          29.09 
_reflns_number_total              13290 
_reflns_number_gt                 6076 
_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)+(0.0638P)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          13290 
_refine_ls_number_parameters      667 
_refine_ls_number_restraints      5 
_refine_ls_R_factor_all           0.1646 
_refine_ls_R_factor_gt            0.0555 
_refine_ls_wR_factor_ref          0.1593 
_refine_ls_wR_factor_gt           0.1356 
_refine_ls_goodness_of_fit_ref    0.942 
_refine_ls_restrained_S_all       0.945 
_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 
C301 C 0.6532(18) 0.2232(11) 0.2477(17) 0.259(13) Uiso 0.898(16) 1 d PD A 1 
C302 C 0.617(2) 0.2922(13) 0.2661(17) 0.304(17) Uiso 0.898(16) 1 d PD A 1 
C303 C 0.639(2) 0.3571(13) 0.2421(18) 0.317(17) Uiso 0.898(16) 1 d PD A 1 
C304 C 0.664(2) 0.4278(13) 0.259(2) 0.36(2) Uiso 0.898(16) 1 d PD A 1 
Si1 Si 0.32535(16) 0.42104(10) -0.05644(12) 0.0118(4) Uani 1 1 d . . . 
Si2 Si 0.17350(17) 0.31097(11) -0.03013(10) 0.0137(5) Uani 1 1 d . . . 
Si3 Si -0.04525(15) 0.27943(10) -0.06227(12) 0.0141(5) Uani 1 1 d . . . 
Si4 Si -0.03372(15) 0.12323(10) -0.06259(12) 0.0134(5) Uani 1 1 d . . . 
Si5 Si 0.17881(18) 0.07489(10) -0.02809(10) 0.0124(5) Uani 1 1 d . . . 
Si6 Si 0.31944(15) 0.19190(10) -0.05674(12) 0.0132(4) Uani 1 1 d . . . 
Si7 Si 0.32223(18) 0.42431(10) 0.17140(11) 0.0128(5) Uani 1 1 d . . . 
Si8 Si 0.17935(16) 0.31016(11) 0.12750(10) 0.0135(5) Uani 1 1 d . . . 
Si9 Si -0.03277(16) 0.27404(10) 0.17522(10) 0.0120(5) Uani 1 1 d . . . 
Si10 Si -0.03080(17) 0.11982(11) 0.17548(10) 0.0138(5) Uani 1 1 d . . . 
Si11 Si 0.17942(17) 0.07113(10) 0.12988(11) 0.0129(5) Uani 1 1 d . . . 
Si12 Si 0.31791(17) 0.18878(11) 0.16795(10) 0.0131(5) Uani 1 1 d . . . 
Si13 Si 0.33643(15) 0.42678(9) 0.55807(13) 0.0124(5) Uani 1 1 d . . . 
Si14 Si 0.19105(16) 0.31071(11) 0.52813(10) 0.0138(5) Uani 1 1 d . . . 
Si15 Si -0.02862(15) 0.27841(10) 0.56143(12) 0.0123(5) Uani 1 1 d . . . 
Si16 Si -0.03113(15) 0.12174(10) 0.56361(11) 0.0117(5) Uani 1 1 d . . . 
Si17 Si 0.18220(17) 0.07062(10) 0.52773(10) 0.0104(5) Uani 1 1 d . . . 
Si18 Si 0.32271(16) 0.18639(10) 0.56185(11) 0.0123(5) Uani 1 1 d . . . 
Si19 Si 0.31864(17) 0.42373(10) 0.32770(11) 0.0126(5) Uani 1 1 d . . . 
Si20 Si 0.17623(17) 0.31099(11) 0.36972(11) 0.0139(5) Uani 1 1 d . . . 
Si21 Si -0.03885(16) 0.27374(11) 0.33052(11) 0.0138(5) Uani 1 1 d . . . 
Si22 Si -0.03475(17) 0.11932(11) 0.32931(11) 0.0137(5) Uani 1 1 d . . . 
Si23 Si 0.17955(18) 0.07140(9) 0.36971(11) 0.0128(5) Uani 1 1 d . . . 
Si24 Si 0.30631(16) 0.19147(10) 0.32185(10) 0.0125(5) Uani 1 1 d . . . 
O1 O 0.2272(4) 0.3756(2) -0.0562(3) 0.0327(15) Uani 1 1 d . . . 
O2 O 0.0659(4) 0.3079(2) -0.0635(3) 0.0247(13) Uani 1 1 d . . . 
O3 O -0.0437(4) 0.2008(2) -0.0525(3) 0.0424(15) Uani 1 1 d . . . 
O4 O 0.0804(4) 0.1028(3) -0.0643(3) 0.0265(14) Uani 1 1 d . . . 
O5 O 0.2730(4) 0.1194(3) -0.0486(3) 0.0275(14) Uani 1 1 d . . . 
O6 O 0.2341(4) 0.2463(3) -0.0493(3) 0.0380(16) Uani 1 1 d . . . 
O7 O 0.2334(5) 0.3748(3) 0.1550(3) 0.0353(18) Uani 1 1 d . . . 
O8 O 0.0734(4) 0.3049(3) 0.1645(3) 0.0321(15) Uani 1 1 d . . . 
O9 O -0.0306(5) 0.1965(3) 0.1560(2) 0.0304(16) Uani 1 1 d . . . 
O10 O 0.0796(4) 0.0906(3) 0.1673(3) 0.0331(15) Uani 1 1 d . . . 
O11 O 0.2681(4) 0.1195(3) 0.1516(3) 0.0250(15) Uani 1 1 d . . . 
O12 O 0.2455(4) 0.2467(3) 0.1434(3) 0.0378(17) Uani 1 1 d . . . 
O13 O 0.1628(4) 0.3143(3) 0.0492(3) 0.0472(17) Uani 1 1 d . . . 
O14 O 0.1614(4) 0.0772(3) 0.0514(3) 0.0291(13) Uani 1 1 d . . . 
O15 O 0.3832(4) 0.4153(3) -0.1258(3) 0.0330(16) Uani 1 1 d . . . 
O16 O 0.3962(5) 0.3990(3) 0.0031(3) 0.0386(17) Uani 1 1 d . . . 
O17 O 0.4213(4) 0.4011(3) 0.1328(3) 0.0268(15) Uani 1 1 d . . . 
O18 O 0.3675(4) 0.1969(3) -0.1294(3) 0.0254(13) Uani 1 1 d . . . 
O19 O 0.4051(4) 0.2034(3) -0.0018(3) 0.0333(15) Uani 1 1 d . . . 
O20 O 0.4209(4) 0.1954(3) 0.1281(3) 0.0266(14) Uani 1 1 d . . . 
O21 O 0.2031(4) 0.0012(2) -0.0530(3) 0.0210(13) Uani 1 1 d . . . 
O22 O 0.2103(4) -0.0029(3) 0.1499(3) 0.0250(15) Uani 1 1 d . . . 
O23 O 0.3459(3) 0.4222(2) 0.2502(3) 0.0297(11) Uani 1 1 d . . . 
O24 O 0.3421(3) 0.1954(2) 0.2460(3) 0.0256(11) Uani 1 1 d . . . 
O25 O -0.0603(3) 0.28355(19) 0.2519(3) 0.0232(10) Uani 1 1 d . . . 
O26 O -0.0645(3) 0.11060(18) 0.2509(3) 0.0217(10) Uani 1 1 d . . . 
O27 O 0.2438(4) 0.3768(3) 0.5549(4) 0.0347(15) Uani 1 1 d . . . 
O28 O 0.0780(4) 0.3115(2) 0.5542(3) 0.0285(13) Uani 1 1 d . . . 
O29 O -0.0160(4) 0.1994(2) 0.5649(3) 0.0388(16) Uani 1 1 d . . . 
O30 O 0.0729(4) 0.0862(3) 0.5563(3) 0.0330(14) Uani 1 1 d . . . 
O31 O 0.2629(4) 0.1189(2) 0.5613(3) 0.0247(13) Uani 1 1 d . . . 
O32 O 0.2478(4) 0.2476(3) 0.5581(3) 0.0301(14) Uani 1 1 d . . . 
O33 O 0.2258(4) 0.3772(3) 0.3418(3) 0.0273(16) Uani 1 1 d . . . 
O34 O 0.0596(4) 0.3117(2) 0.3526(2) 0.0235(14) Uani 1 1 d . . . 
O35 O -0.0251(5) 0.1962(2) 0.3478(2) 0.0298(16) Uani 1 1 d . . . 
O36 O 0.0692(5) 0.0861(3) 0.3439(3) 0.0432(19) Uani 1 1 d . . . 
O37 O 0.2561(5) 0.1208(3) 0.3335(3) 0.0379(17) Uani 1 1 d . . . 
O38 O 0.2251(5) 0.2471(3) 0.3344(3) 0.0364(16) Uani 1 1 d . . . 
O39 O 0.1937(4) 0.3059(3) 0.4485(3) 0.0487(16) Uani 1 1 d . . . 
O40 O 0.1835(4) 0.0819(2) 0.4489(3) 0.0336(14) Uani 1 1 d . . . 
O41 O 0.3902(4) 0.4187(3) 0.6290(3) 0.0321(16) Uani 1 1 d . . . 
O42 O 0.4138(4) 0.4126(3) 0.4991(3) 0.0315(15) Uani 1 1 d . . . 
O43 O 0.4139(4) 0.3986(3) 0.3685(3) 0.0287(15) Uani 1 1 d . . . 
O44 O 0.3865(4) 0.1889(3) 0.6299(3) 0.0232(13) Uani 1 1 d . . . 
O45 O 0.3953(4) 0.1873(3) 0.4986(3) 0.0296(14) Uani 1 1 d . . . 
O46 O -0.0979(4) 0.2975(3) -0.1313(3) 0.0356(16) Uani 1 1 d . . . 
O47 O 0.2105(4) -0.0049(2) 0.5447(3) 0.0210(14) Uani 1 1 d . . . 
O48 O 0.2093(4) -0.0030(3) 0.3512(3) 0.0284(15) 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 1.522(17) . ? 
C302 C303 1.429(17) . ? 
C303 C304 1.509(18) . ? 
Si1 O16 1.588(6) . ? 
Si1 O47 1.589(5) 2 ? 
Si1 O15 1.596(6) . ? 
Si1 O1 1.609(5) . ? 
Si2 O1 1.581(5) . ? 
Si2 O6 1.587(6) . ? 
Si2 O13 1.593(6) . ? 
Si2 O2 1.595(5) . ? 
Si3 O46 1.593(6) . ? 
Si3 O3 1.600(5) . ? 
Si3 O2 1.603(5) . ? 
Si3 O45 1.604(6) 4_565 ? 
Si4 O3 1.586(5) . ? 
Si4 O4 1.591(5) . ? 
Si4 O42 1.595(6) 4_565 ? 
Si4 O43 1.608(6) 4_565 ? 
Si5 O21 1.603(5) . ? 
Si5 O14 1.608(6) . ? 
Si5 O5 1.608(5) . ? 
Si5 O4 1.610(5) . ? 
Si6 O18 1.595(6) . ? 
Si6 O6 1.597(5) . ? 
Si6 O5 1.601(5) . ? 
Si6 O19 1.608(5) . ? 
Si7 O7 1.592(6) . ? 
Si7 O48 1.593(6) 2 ? 
Si7 O23 1.607(7) . ? 
Si7 O17 1.612(6) . ? 
Si8 O13 1.584(6) . ? 
Si8 O12 1.592(6) . ? 
Si8 O7 1.593(6) . ? 
Si8 O8 1.612(6) . ? 
Si9 O8 1.573(5) . ? 
Si9 O25 1.589(6) . ? 
Si9 O44 1.599(5) 4_565 ? 
Si9 O9 1.613(5) . ? 
Si10 O26 1.587(6) . ? 
Si10 O9 1.597(6) . ? 
Si10 O10 1.608(6) . ? 
Si10 O41 1.613(6) 4_565 ? 
Si11 O10 1.589(6) . ? 
Si11 O14 1.591(6) . ? 
Si11 O22 1.601(6) . ? 
Si11 O11 1.602(6) . ? 
Si12 O11 1.586(6) . ? 
Si12 O24 1.600(6) . ? 
Si12 O12 1.600(6) . ? 
Si12 O20 1.605(5) . ? 
Si13 O21 1.597(5) 2 ? 
Si13 O41 1.598(6) . ? 
Si13 O42 1.601(6) . ? 
Si13 O27 1.605(5) . ? 
Si14 O39 1.595(6) . ? 
Si14 O32 1.601(5) . ? 
Si14 O27 1.605(6) . ? 
Si14 O28 1.610(5) . ? 
Si15 O20 1.588(5) 4_566 ? 
Si15 O19 1.589(5) 4_566 ? 
Si15 O28 1.590(5) . ? 
Si15 O29 1.607(5) . ? 
Si16 O30 1.581(5) . ? 
Si16 O29 1.581(5) . ? 
Si16 O17 1.593(6) 4_566 ? 
Si16 O16 1.610(6) 4_566 ? 
Si17 O40 1.592(6) . ? 
Si17 O31 1.607(5) . ? 
Si17 O47 1.609(5) . ? 
Si17 O30 1.610(6) . ? 
Si18 O31 1.582(5) . ? 
Si18 O32 1.598(5) . ? 
Si18 O45 1.600(6) . ? 
Si18 O44 1.608(5) . ? 
Si19 O33 1.589(6) . ? 
Si19 O23 1.593(7) . ? 
Si19 O22 1.597(6) 2 ? 
Si19 O43 1.601(6) . ? 
Si20 O39 1.595(6) . ? 
Si20 O33 1.596(6) . ? 
Si20 O34 1.606(6) . ? 
Si20 O38 1.611(5) . ? 
Si21 O34 1.594(5) . ? 
Si21 O18 1.607(6) 4_566 ? 
Si21 O25 1.610(6) . ? 
Si21 O35 1.613(5) . ? 
Si22 O36 1.579(6) . ? 
Si22 O15 1.586(6) 4_566 ? 
Si22 O35 1.602(5) . ? 
Si22 O26 1.627(6) . ? 
Si23 O40 1.598(6) . ? 
Si23 O48 1.599(6) . ? 
Si23 O36 1.600(6) . ? 
Si23 O37 1.607(6) . ? 
Si24 O38 1.589(6) . ? 
Si24 O24 1.593(6) . ? 
Si24 O37 1.596(6) . ? 
Si24 O46 1.608(6) 4_666 ? 
O15 Si22 1.586(6) 4_665 ? 
O16 Si16 1.610(6) 4_665 ? 
O17 Si16 1.593(6) 4_665 ? 
O18 Si21 1.607(6) 4_665 ? 
O19 Si15 1.589(5) 4_665 ? 
O20 Si15 1.588(5) 4_665 ? 
O21 Si13 1.597(5) 2_545 ? 
O22 Si19 1.598(6) 2_545 ? 
O41 Si10 1.612(6) 4_666 ? 
O42 Si4 1.596(6) 4_666 ? 
O43 Si4 1.608(6) 4_666 ? 
O44 Si9 1.599(5) 4_666 ? 
O45 Si3 1.604(6) 4_666 ? 
O46 Si24 1.608(6) 4_565 ? 
O47 Si1 1.589(5) 2_545 ? 
O48 Si7 1.593(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 
C303 C302 C301 134(3) . . ? 
C302 C303 C304 147(4) . . ? 
O16 Si1 O47 109.6(3) . 2 ? 
O16 Si1 O15 109.7(3) . . ? 
O47 Si1 O15 110.3(3) 2 . ? 
O16 Si1 O1 109.3(3) . . ? 
O47 Si1 O1 106.7(3) 2 . ? 
O15 Si1 O1 111.3(4) . . ? 
O1 Si2 O6 111.4(3) . . ? 
O1 Si2 O13 109.6(4) . . ? 
O6 Si2 O13 108.8(3) . . ? 
O1 Si2 O2 108.0(3) . . ? 
O6 Si2 O2 109.5(3) . . ? 
O13 Si2 O2 109.5(3) . . ? 
O46 Si3 O3 109.9(4) . . ? 
O46 Si3 O2 108.6(3) . . ? 
O3 Si3 O2 110.2(3) . . ? 
O46 Si3 O45 109.8(3) . 4_565 ? 
O3 Si3 O45 109.2(3) . 4_565 ? 
O2 Si3 O45 109.1(3) . 4_565 ? 
O3 Si4 O4 109.9(3) . . ? 
O3 Si4 O42 108.2(3) . 4_565 ? 
O4 Si4 O42 109.1(3) . 4_565 ? 
O3 Si4 O43 110.0(3) . 4_565 ? 
O4 Si4 O43 109.4(3) . 4_565 ? 
O42 Si4 O43 110.1(3) 4_565 4_565 ? 
O21 Si5 O14 111.3(3) . . ? 
O21 Si5 O5 106.2(3) . . ? 
O14 Si5 O5 110.6(3) . . ? 
O21 Si5 O4 110.7(3) . . ? 
O14 Si5 O4 108.2(3) . . ? 
O5 Si5 O4 109.8(3) . . ? 
O18 Si6 O6 109.5(3) . . ? 
O18 Si6 O5 108.1(3) . . ? 
O6 Si6 O5 109.8(3) . . ? 
O18 Si6 O19 108.8(3) . . ? 
O6 Si6 O19 110.6(4) . . ? 
O5 Si6 O19 110.0(3) . . ? 
O7 Si7 O48 108.7(3) . 2 ? 
O7 Si7 O23 109.5(3) . . ? 
O48 Si7 O23 110.8(3) 2 . ? 
O7 Si7 O17 109.9(3) . . ? 
O48 Si7 O17 110.6(3) 2 . ? 
O23 Si7 O17 107.4(3) . . ? 
O13 Si8 O12 108.5(3) . . ? 
O13 Si8 O7 111.2(3) . . ? 
O12 Si8 O7 109.6(3) . . ? 
O13 Si8 O8 109.6(3) . . ? 
O12 Si8 O8 110.5(3) . . ? 
O7 Si8 O8 107.5(3) . . ? 
O8 Si9 O25 107.2(3) . . ? 
O8 Si9 O44 110.8(3) . 4_565 ? 
O25 Si9 O44 109.3(3) . 4_565 ? 
O8 Si9 O9 109.6(3) . . ? 
O25 Si9 O9 110.6(3) . . ? 
O44 Si9 O9 109.4(3) 4_565 . ? 
O26 Si10 O9 110.3(3) . . ? 
O26 Si10 O10 108.6(3) . . ? 
O9 Si10 O10 109.3(3) . . ? 
O26 Si10 O41 107.6(3) . 4_565 ? 
O9 Si10 O41 109.2(3) . 4_565 ? 
O10 Si10 O41 111.9(4) . 4_565 ? 
O10 Si11 O14 108.5(3) . . ? 
O10 Si11 O22 109.4(3) . . ? 
O14 Si11 O22 110.9(3) . . ? 
O10 Si11 O11 110.6(3) . . ? 
O14 Si11 O11 109.4(3) . . ? 
O22 Si11 O11 107.9(3) . . ? 
O11 Si12 O24 111.1(3) . . ? 
O11 Si12 O12 109.0(3) . . ? 
O24 Si12 O12 111.1(3) . . ? 
O11 Si12 O20 109.6(3) . . ? 
O24 Si12 O20 107.6(3) . . ? 
O12 Si12 O20 108.3(3) . . ? 
O21 Si13 O41 107.6(3) 2 . ? 
O21 Si13 O42 109.8(3) 2 . ? 
O41 Si13 O42 109.9(3) . . ? 
O21 Si13 O27 109.3(3) 2 . ? 
O41 Si13 O27 108.7(4) . . ? 
O42 Si13 O27 111.4(3) . . ? 
O39 Si14 O32 108.3(3) . . ? 
O39 Si14 O27 111.9(3) . . ? 
O32 Si14 O27 109.1(3) . . ? 
O39 Si14 O28 110.3(3) . . ? 
O32 Si14 O28 109.7(3) . . ? 
O27 Si14 O28 107.6(3) . . ? 
O20 Si15 O19 110.5(3) 4_566 4_566 ? 
O20 Si15 O28 108.9(3) 4_566 . ? 
O19 Si15 O28 109.7(3) 4_566 . ? 
O20 Si15 O29 109.9(3) 4_566 . ? 
O19 Si15 O29 108.9(3) 4_566 . ? 
O28 Si15 O29 109.1(3) . . ? 
O30 Si16 O29 109.7(3) . . ? 
O30 Si16 O17 107.8(3) . 4_566 ? 
O29 Si16 O17 109.0(3) . 4_566 ? 
O30 Si16 O16 110.5(4) . 4_566 ? 
O29 Si16 O16 110.4(3) . 4_566 ? 
O17 Si16 O16 109.4(3) 4_566 4_566 ? 
O40 Si17 O31 108.6(3) . . ? 
O40 Si17 O47 109.9(3) . . ? 
O31 Si17 O47 109.2(3) . . ? 
O40 Si17 O30 109.5(3) . . ? 
O31 Si17 O30 110.6(3) . . ? 
O47 Si17 O30 109.1(3) . . ? 
O31 Si18 O32 110.2(3) . . ? 
O31 Si18 O45 108.4(3) . . ? 
O32 Si18 O45 109.9(3) . . ? 
O31 Si18 O44 107.7(3) . . ? 
O32 Si18 O44 110.6(3) . . ? 
O45 Si18 O44 110.0(3) . . ? 
O33 Si19 O23 110.1(3) . . ? 
O33 Si19 O22 107.9(3) . 2 ? 
O23 Si19 O22 110.4(3) . 2 ? 
O33 Si19 O43 110.6(3) . . ? 
O23 Si19 O43 107.6(3) . . ? 
O22 Si19 O43 110.3(3) 2 . ? 
O39 Si20 O33 109.8(3) . . ? 
O39 Si20 O34 110.7(3) . . ? 
O33 Si20 O34 109.1(3) . . ? 
O39 Si20 O38 108.7(3) . . ? 
O33 Si20 O38 110.3(3) . . ? 
O34 Si20 O38 108.3(3) . . ? 
O34 Si21 O18 109.7(3) . 4_566 ? 
O34 Si21 O25 111.1(3) . . ? 
O18 Si21 O25 107.5(3) 4_566 . ? 
O34 Si21 O35 108.2(3) . . ? 
O18 Si21 O35 109.9(3) 4_566 . ? 
O25 Si21 O35 110.4(3) . . ? 
O36 Si22 O15 109.0(3) . 4_566 ? 
O36 Si22 O35 107.4(3) . . ? 
O15 Si22 O35 110.7(3) 4_566 . ? 
O36 Si22 O26 110.4(3) . . ? 
O15 Si22 O26 109.1(3) 4_566 . ? 
O35 Si22 O26 110.3(3) . . ? 
O40 Si23 O48 110.3(3) . . ? 
O40 Si23 O36 108.9(3) . . ? 
O48 Si23 O36 109.4(3) . . ? 
O40 Si23 O37 110.1(3) . . ? 
O48 Si23 O37 108.6(3) . . ? 
O36 Si23 O37 109.6(4) . . ? 
O38 Si24 O24 108.9(3) . . ? 
O38 Si24 O37 108.5(4) . . ? 
O24 Si24 O37 108.2(3) . . ? 
O38 Si24 O46 111.2(3) . 4_666 ? 
O24 Si24 O46 107.7(3) . 4_666 ? 
O37 Si24 O46 112.2(3) . 4_666 ? 
Si2 O1 Si1 148.0(4) . . ? 
Si2 O2 Si3 148.7(4) . . ? 
Si4 O3 Si3 165.1(5) . . ? 
Si4 O4 Si5 151.1(4) . . ? 
Si6 O5 Si5 147.8(4) . . ? 
Si2 O6 Si6 163.5(5) . . ? 
Si7 O7 Si8 158.2(5) . . ? 
Si9 O8 Si8 153.3(4) . . ? 
Si10 O9 Si9 152.1(3) . . ? 
Si11 O10 Si10 157.1(4) . . ? 
Si12 O11 Si11 155.3(4) . . ? 
Si8 O12 Si12 172.1(4) . . ? 
Si8 O13 Si2 165.7(4) . . ? 
Si11 O14 Si5 161.8(4) . . ? 
Si22 O15 Si1 149.9(4) 4_665 . ? 
Si1 O16 Si16 178.8(5) . 4_665 ? 
Si16 O17 Si7 146.5(4) 4_665 . ? 
Si6 O18 Si21 142.8(4) . 4_665 ? 
Si15 O19 Si6 167.9(5) 4_665 . ? 
Si15 O20 Si12 144.6(4) 4_665 . ? 
Si13 O21 Si5 145.6(4) 2_545 . ? 
Si19 O22 Si11 150.8(4) 2_545 . ? 
Si19 O23 Si7 155.1(3) . . ? 
Si24 O24 Si12 149.6(3) . . ? 
Si9 O25 Si21 152.3(3) . . ? 
Si10 O26 Si22 146.4(3) . . ? 
Si14 O27 Si13 151.6(4) . . ? 
Si15 O28 Si14 151.5(4) . . ? 
Si16 O29 Si15 166.1(4) . . ? 
Si16 O30 Si17 158.7(4) . . ? 
Si18 O31 Si17 150.4(4) . . ? 
Si18 O32 Si14 159.1(4) . . ? 
Si19 O33 Si20 152.4(4) . . ? 
Si21 O34 Si20 150.1(4) . . ? 
Si22 O35 Si21 151.9(4) . . ? 
Si22 O36 Si23 163.9(5) . . ? 
Si24 O37 Si23 153.3(4) . . ? 
Si24 O38 Si20 156.6(4) . . ? 
Si14 O39 Si20 167.9(4) . . ? 
Si17 O40 Si23 164.0(4) . . ? 
Si13 O41 Si10 149.1(4) . 4_666 ? 
Si4 O42 Si13 160.0(4) 4_666 . ? 
Si19 O43 Si4 150.8(4) . 4_666 ? 
Si9 O44 Si18 148.8(4) 4_666 . ? 
Si18 O45 Si3 155.6(4) . 4_666 ? 
Si3 O46 Si24 153.1(4) . 4_565 ? 
Si1 O47 Si17 148.4(4) 2_545 . ? 
Si7 O48 Si23 149.9(4) 2_545 . ? 
  
_diffrn_measured_fraction_theta_max    0.912 
_diffrn_reflns_theta_full              29.09 
_diffrn_measured_fraction_theta_full   0.912 
_refine_diff_density_max    1.152 
_refine_diff_density_min   -0.791 
_refine_diff_density_rms    0.171 




  
data_f_hexane_twin_24 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C4 O48 Si24' 
_chemical_formula_weight          1490 
  
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                    13.517(6) 
_cell_length_b                    20.307(10) 
_cell_length_c                    20.071(9) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  89.998(6) 
_cell_angle_gamma                 90.00 
_cell_volume                      5509(4) 
_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           0.26 
_exptl_crystal_size_mid           0.13 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.843 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3080 
_exptl_absorpt_coefficient_mu     0.659 
_exptl_absorpt_correction_type    Analytical 
_exptl_absorpt_correction_T_min   0.8468 
_exptl_absorpt_correction_T_max   0.9547 
_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             59220 
_diffrn_reflns_av_R_equivalents   0.0886 
_diffrn_reflns_av_sigmaI/netI     0.0498 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        -25 
_diffrn_reflns_limit_l_max        25 
_diffrn_reflns_theta_min          1.00 
_diffrn_reflns_theta_max          27.61 
_reflns_number_total              12034 
_reflns_number_gt                 10366 
_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)+(0.0832P)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          12034 
_refine_ls_number_parameters      675 
_refine_ls_number_restraints      9 
_refine_ls_R_factor_all           0.0501 
_refine_ls_R_factor_gt            0.0416 
_refine_ls_wR_factor_ref          0.1357 
_refine_ls_wR_factor_gt           0.1302 
_refine_ls_goodness_of_fit_ref    1.069 
_refine_ls_restrained_S_all       1.079 
_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 
C306 C 0.225(2) 0.0477(12) 0.7487(14) 0.307(16) Uiso 0.67(2) 1 d PD A 1 
C305 C 0.141(3) 0.0960(15) 0.755(2) 0.48(3) Uiso 0.67(2) 1 d PD A 1 
C304 C 0.149(3) 0.1707(14) 0.7491(19) 0.39(2) Uiso 0.67(2) 1 d PD A 1 
C303 C 0.118(2) 0.2422(15) 0.7579(17) 0.40(2) Uiso 0.67(2) 1 d PD A 1 
C302 C 0.174(2) 0.3078(15) 0.7489(17) 0.308(18) Uiso 0.67(2) 1 d PD A 1 
C301 C 0.134(5) 0.3799(18) 0.745(2) 0.69(5) Uiso 0.67(2) 1 d PD A 1 
Si1 Si 0.32466(7) 0.42089(4) -0.05675(5) 0.01296(19) Uani 1 1 d . . . 
Si2 Si 0.17236(8) 0.31119(4) -0.03033(5) 0.0149(2) Uani 1 1 d . . . 
Si3 Si -0.04637(7) 0.27948(4) -0.06188(5) 0.0144(2) Uani 1 1 d . . . 
Si4 Si -0.03386(7) 0.12334(4) -0.06249(4) 0.01350(19) Uani 1 1 d . . . 
Si5 Si 0.17901(7) 0.07497(4) -0.02829(4) 0.01239(19) Uani 1 1 d . . . 
Si6 Si 0.31864(7) 0.19217(4) -0.05719(5) 0.0139(2) Uani 1 1 d . . . 
Si7 Si 0.32224(8) 0.42425(4) 0.17161(4) 0.01367(19) Uani 1 1 d . . . 
Si8 Si 0.17866(8) 0.31033(4) 0.12765(5) 0.0139(2) Uani 1 1 d . . . 
Si9 Si -0.03317(7) 0.27393(4) 0.17526(4) 0.0135(2) Uani 1 1 d . . . 
Si10 Si -0.03094(7) 0.11973(4) 0.17550(4) 0.0144(2) Uani 1 1 d . . . 
Si11 Si 0.17921(7) 0.07097(4) 0.12966(5) 0.01319(19) Uani 1 1 d . . . 
Si12 Si 0.31726(8) 0.18914(4) 0.16772(5) 0.0134(2) Uani 1 1 d . . . 
Si13 Si 0.33601(7) 0.42655(4) 0.55797(5) 0.01264(19) Uani 1 1 d . . . 
Si14 Si 0.18992(8) 0.31090(4) 0.52815(5) 0.0140(2) Uani 1 1 d . . . 
Si15 Si -0.02915(7) 0.27802(4) 0.56118(5) 0.01319(19) Uani 1 1 d . . . 
Si16 Si -0.03149(7) 0.12168(4) 0.56357(4) 0.01293(19) Uani 1 1 d . . . 
Si17 Si 0.18166(7) 0.07064(4) 0.52781(4) 0.01178(19) Uani 1 1 d . . . 
Si18 Si 0.32165(8) 0.18696(4) 0.56201(5) 0.0139(2) Uani 1 1 d . . . 
Si19 Si 0.31853(7) 0.42360(4) 0.32760(4) 0.0134(2) Uani 1 1 d . . . 
Si20 Si 0.17549(8) 0.31096(4) 0.36967(5) 0.0146(2) Uani 1 1 d . . . 
Si21 Si -0.03960(7) 0.27368(4) 0.33050(4) 0.0142(2) Uani 1 1 d . . . 
Si22 Si -0.03459(7) 0.11947(4) 0.32934(4) 0.0146(2) Uani 1 1 d . . . 
Si23 Si 0.17990(8) 0.07135(4) 0.36968(5) 0.01350(19) Uani 1 1 d . . . 
Si24 Si 0.30547(8) 0.19136(4) 0.32172(4) 0.0134(2) Uani 1 1 d . . . 
O1 O 0.2271(2) 0.37557(12) -0.05817(15) 0.0348(7) Uani 1 1 d . . . 
O2 O 0.0643(2) 0.30835(11) -0.06355(14) 0.0280(6) Uani 1 1 d . . . 
O3 O -0.0428(3) 0.20092(11) -0.05061(17) 0.0425(8) Uani 1 1 d . . . 
O4 O 0.08058(18) 0.10237(13) -0.06487(12) 0.0269(6) Uani 1 1 d . . . 
O5 O 0.27251(19) 0.12007(11) -0.04775(14) 0.0268(6) Uani 1 1 d . . . 
O6 O 0.2329(2) 0.24624(12) -0.05015(16) 0.0387(7) Uani 1 1 d . . . 
O7 O 0.2329(2) 0.37508(14) 0.15453(15) 0.0385(8) Uani 1 1 d . . . 
O8 O 0.0737(2) 0.30564(13) 0.16358(16) 0.0360(7) Uani 1 1 d . . . 
O9 O -0.0291(3) 0.19650(11) 0.15531(13) 0.0337(8) Uani 1 1 d . . . 
O10 O 0.0791(2) 0.09041(14) 0.16766(14) 0.0365(7) Uani 1 1 d . . . 
O11 O 0.2672(2) 0.11899(13) 0.15269(13) 0.0335(7) Uani 1 1 d . . . 
O12 O 0.2430(2) 0.24640(13) 0.14356(14) 0.0406(8) Uani 1 1 d . . . 
O13 O 0.1620(3) 0.31497(15) 0.04928(14) 0.0514(9) Uani 1 1 d . . . 
O14 O 0.1616(2) 0.07698(13) 0.05096(12) 0.0328(6) Uani 1 1 d . . . 
O15 O 0.3807(2) 0.41477(13) -0.12628(13) 0.0340(7) Uani 1 1 d . . . 
O16 O 0.3957(2) 0.39711(15) 0.00303(13) 0.0409(8) Uani 1 1 d . . . 
O17 O 0.42115(19) 0.40174(13) 0.13273(12) 0.0286(6) Uani 1 1 d . . . 
O18 O 0.3670(2) 0.19681(12) -0.12960(13) 0.0264(6) Uani 1 1 d . . . 
O19 O 0.4039(2) 0.20432(15) -0.00204(14) 0.0382(8) Uani 1 1 d . . . 
O20 O 0.4205(2) 0.19524(12) 0.12807(13) 0.0279(6) Uani 1 1 d . . . 
O21 O 0.20434(18) 0.00120(10) -0.05258(13) 0.0232(5) Uani 1 1 d . . . 
O22 O 0.2098(2) -0.00300(12) 0.14915(13) 0.0297(6) Uani 1 1 d . . . 
O23 O 0.34635(19) 0.42253(13) 0.25011(14) 0.0341(6) Uani 1 1 d . . . 
O24 O 0.3417(2) 0.19555(11) 0.24627(13) 0.0277(6) Uani 1 1 d . . . 
O25 O -0.06204(18) 0.28317(11) 0.25217(12) 0.0251(5) Uani 1 1 d . . . 
O26 O -0.06378(17) 0.11044(11) 0.25179(12) 0.0235(5) Uani 1 1 d . . . 
O27 O 0.2429(2) 0.37741(12) 0.55274(16) 0.0375(7) Uani 1 1 d . . . 
O28 O 0.0772(2) 0.31242(11) 0.55353(15) 0.0273(6) Uani 1 1 d . . . 
O29 O -0.0137(3) 0.19913(11) 0.56522(17) 0.0417(8) Uani 1 1 d . . . 
O30 O 0.07214(19) 0.08533(13) 0.55515(15) 0.0367(7) Uani 1 1 d . . . 
O31 O 0.26029(19) 0.11866(11) 0.56295(12) 0.0267(6) Uani 1 1 d . . . 
O32 O 0.2459(2) 0.24844(12) 0.55890(14) 0.0329(7) Uani 1 1 d . . . 
O33 O 0.2252(2) 0.37681(12) 0.34169(14) 0.0325(7) Uani 1 1 d . . . 
O34 O 0.0588(2) 0.31257(11) 0.35328(14) 0.0266(6) Uani 1 1 d . . . 
O35 O -0.0258(3) 0.19631(11) 0.34841(13) 0.0303(7) Uani 1 1 d . . . 
O36 O 0.0697(2) 0.08484(15) 0.34357(15) 0.0436(8) Uani 1 1 d . . . 
O37 O 0.2564(2) 0.12035(13) 0.33459(14) 0.0380(8) Uani 1 1 d . . . 
O38 O 0.2240(2) 0.24721(13) 0.33420(15) 0.0369(7) Uani 1 1 d . . . 
O39 O 0.1930(3) 0.30587(14) 0.44863(14) 0.0477(9) Uani 1 1 d . . . 
O40 O 0.1841(2) 0.08245(12) 0.44889(12) 0.0355(7) Uani 1 1 d . . . 
O41 O 0.3913(2) 0.41780(13) 0.62865(13) 0.0327(7) Uani 1 1 d . . . 
O42 O 0.4140(2) 0.41303(13) 0.49950(13) 0.0313(6) Uani 1 1 d . . . 
O43 O 0.41458(19) 0.39737(14) 0.36824(12) 0.0303(6) Uani 1 1 d . . . 
O44 O 0.3852(2) 0.18961(11) 0.63006(13) 0.0271(6) Uani 1 1 d . . . 
O45 O 0.3942(2) 0.18830(12) 0.49902(14) 0.0320(7) Uani 1 1 d . . . 
O46 O -0.0996(2) 0.29764(15) -0.13096(14) 0.0393(8) Uani 1 1 d . . . 
O47 O 0.21034(19) -0.00435(11) 0.54567(13) 0.0261(6) Uani 1 1 d . . . 
O48 O 0.2104(2) -0.00276(12) 0.35094(13) 0.0312(6) 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 
C306 C305 1.511(19) . ? 
C305 C304 1.527(18) . ? 
C304 C303 1.524(17) . ? 
C303 C302 1.546(18) . ? 
C302 C301 1.565(19) . ? 
Si1 O15 1.593(3) . ? 
Si1 O47 1.606(2) 2 ? 
Si1 O1 1.608(3) . ? 
Si1 O16 1.611(3) . ? 
Si2 O6 1.602(3) . ? 
Si2 O1 1.603(3) . ? 
Si2 O13 1.606(3) . ? 
Si2 O2 1.607(3) . ? 
Si3 O45 1.602(3) 4_565 ? 
Si3 O46 1.605(3) . ? 
Si3 O2 1.606(3) . ? 
Si3 O3 1.612(3) . ? 
Si4 O3 1.598(3) . ? 
Si4 O4 1.605(3) . ? 
Si4 O42 1.609(3) 4_565 ? 
Si4 O43 1.611(3) 4_565 ? 
Si5 O14 1.608(3) . ? 
Si5 O5 1.609(2) . ? 
Si5 O21 1.612(2) . ? 
Si5 O4 1.618(3) . ? 
Si6 O18 1.596(3) . ? 
Si6 O6 1.603(3) . ? 
Si6 O5 1.603(2) . ? 
Si6 O19 1.617(3) . ? 
Si7 O7 1.605(3) . ? 
Si7 O23 1.609(3) . ? 
Si7 O48 1.612(3) 2 ? 
Si7 O17 1.614(3) . ? 
Si8 O13 1.592(3) . ? 
Si8 O8 1.595(3) . ? 
Si8 O12 1.595(3) . ? 
Si8 O7 1.599(3) . ? 
Si9 O8 1.599(3) . ? 
Si9 O25 1.603(3) . ? 
Si9 O44 1.609(3) 4_565 ? 
Si9 O9 1.623(3) . ? 
Si10 O41 1.603(3) 4_565 ? 
Si10 O26 1.605(3) . ? 
Si10 O10 1.610(3) . ? 
Si10 O9 1.611(3) . ? 
Si11 O14 1.602(3) . ? 
Si11 O10 1.603(3) . ? 
Si11 O11 1.606(3) . ? 
Si11 O22 1.606(3) . ? 
Si12 O11 1.606(3) . ? 
Si12 O20 1.611(3) . ? 
Si12 O12 1.611(3) . ? 
Si12 O24 1.616(3) . ? 
Si13 O42 1.601(3) . ? 
Si13 O27 1.609(3) . ? 
Si13 O41 1.613(3) . ? 
Si13 O21 1.615(2) 2 ? 
Si14 O39 1.600(3) . ? 
Si14 O32 1.601(3) . ? 
Si14 O27 1.607(3) . ? 
Si14 O28 1.607(3) . ? 
Si15 O19 1.599(3) 4_566 ? 
Si15 O20 1.600(3) 4_566 ? 
Si15 O28 1.605(3) . ? 
Si15 O29 1.618(3) . ? 
Si16 O29 1.591(3) . ? 
Si16 O30 1.592(3) . ? 
Si16 O17 1.601(3) 4_566 ? 
Si16 O16 1.610(3) 4_566 ? 
Si17 O40 1.602(3) . ? 
Si17 O31 1.606(2) . ? 
Si17 O30 1.607(3) . ? 
Si17 O47 1.612(2) . ? 
Si18 O45 1.600(3) . ? 
Si18 O44 1.615(3) . ? 
Si18 O32 1.616(3) . ? 
Si18 O31 1.616(2) . ? 
Si19 O23 1.600(3) . ? 
Si19 O33 1.604(3) . ? 
Si19 O22 1.608(3) 2 ? 
Si19 O43 1.623(3) . ? 
Si20 O33 1.599(3) . ? 
Si20 O39 1.606(3) . ? 
Si20 O34 1.612(3) . ? 
Si20 O38 1.617(3) . ? 
Si21 O18 1.610(3) 4_566 ? 
Si21 O25 1.613(3) . ? 
Si21 O34 1.613(3) . ? 
Si21 O35 1.623(3) . ? 
Si22 O36 1.601(3) . ? 
Si22 O15 1.609(3) 4_566 ? 
Si22 O35 1.611(3) . ? 
Si22 O26 1.616(3) . ? 
Si23 O37 1.599(3) . ? 
Si23 O36 1.603(3) . ? 
Si23 O48 1.605(3) . ? 
Si23 O40 1.607(3) . ? 
Si24 O24 1.594(3) . ? 
Si24 O38 1.600(3) . ? 
Si24 O37 1.608(3) . ? 
Si24 O46 1.612(3) 4_666 ? 
O15 Si22 1.609(3) 4_665 ? 
O16 Si16 1.610(3) 4_665 ? 
O17 Si16 1.601(3) 4_665 ? 
O18 Si21 1.611(3) 4_665 ? 
O19 Si15 1.599(3) 4_665 ? 
O20 Si15 1.600(3) 4_665 ? 
O21 Si13 1.615(2) 2_545 ? 
O22 Si19 1.608(3) 2_545 ? 
O41 Si10 1.603(3) 4_666 ? 
O42 Si4 1.609(3) 4_666 ? 
O43 Si4 1.611(3) 4_666 ? 
O44 Si9 1.609(3) 4_666 ? 
O45 Si3 1.602(3) 4_666 ? 
O46 Si24 1.612(3) 4_565 ? 
O47 Si1 1.606(2) 2_545 ? 
O48 Si7 1.611(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 
C306 C305 C304 126(3) . . ? 
C303 C304 C305 156(3) . . ? 
C304 C303 C302 132(3) . . ? 
C303 C302 C301 130(3) . . ? 
O15 Si1 O47 109.58(14) . 2 ? 
O15 Si1 O1 109.26(16) . . ? 
O47 Si1 O1 107.59(14) 2 . ? 
O15 Si1 O16 110.22(16) . . ? 
O47 Si1 O16 110.85(15) 2 . ? 
O1 Si1 O16 109.29(16) . . ? 
O6 Si2 O1 110.41(17) . . ? 
O6 Si2 O13 109.31(17) . . ? 
O1 Si2 O13 110.36(17) . . ? 
O6 Si2 O2 109.39(15) . . ? 
O1 Si2 O2 107.74(14) . . ? 
O13 Si2 O2 109.59(18) . . ? 
O45 Si3 O46 109.90(18) 4_565 . ? 
O45 Si3 O2 109.50(16) 4_565 . ? 
O46 Si3 O2 108.38(16) . . ? 
O45 Si3 O3 108.18(17) 4_565 . ? 
O46 Si3 O3 111.22(18) . . ? 
O2 Si3 O3 109.64(16) . . ? 
O3 Si4 O4 109.80(16) . . ? 
O3 Si4 O42 107.69(17) . 4_565 ? 
O4 Si4 O42 108.85(15) . 4_565 ? 
O3 Si4 O43 110.70(17) . 4_565 ? 
O4 Si4 O43 108.79(14) . 4_565 ? 
O42 Si4 O43 110.98(15) 4_565 4_565 ? 
O14 Si5 O5 109.89(15) . . ? 
O14 Si5 O21 110.71(13) . . ? 
O5 Si5 O21 106.79(13) . . ? 
O14 Si5 O4 108.65(14) . . ? 
O5 Si5 O4 109.88(14) . . ? 
O21 Si5 O4 110.91(14) . . ? 
O18 Si6 O6 109.64(16) . . ? 
O18 Si6 O5 108.72(14) . . ? 
O6 Si6 O5 109.52(15) . . ? 
O18 Si6 O19 108.79(17) . . ? 
O6 Si6 O19 110.52(17) . . ? 
O5 Si6 O19 109.62(15) . . ? 
O7 Si7 O23 110.37(16) . . ? 
O7 Si7 O48 107.84(16) . 2 ? 
O23 Si7 O48 110.52(14) . 2 ? 
O7 Si7 O17 110.13(15) . . ? 
O23 Si7 O17 107.42(14) . . ? 
O48 Si7 O17 110.57(15) 2 . ? 
O13 Si8 O8 108.95(19) . . ? 
O13 Si8 O12 108.85(16) . . ? 
O8 Si8 O12 110.25(16) . . ? 
O13 Si8 O7 110.46(17) . . ? 
O8 Si8 O7 107.71(16) . . ? 
O12 Si8 O7 110.61(19) . . ? 
O8 Si9 O25 108.29(15) . . ? 
O8 Si9 O44 110.57(17) . 4_565 ? 
O25 Si9 O44 108.80(14) . 4_565 ? 
O8 Si9 O9 108.87(16) . . ? 
O25 Si9 O9 111.05(13) . . ? 
O44 Si9 O9 109.26(15) 4_565 . ? 
O41 Si10 O26 108.80(14) 4_565 . ? 
O41 Si10 O10 111.90(17) 4_565 . ? 
O26 Si10 O10 107.77(14) . . ? 
O41 Si10 O9 108.82(16) 4_565 . ? 
O26 Si10 O9 110.97(13) . . ? 
O10 Si10 O9 108.61(17) . . ? 
O14 Si11 O10 108.97(16) . . ? 
O14 Si11 O11 110.32(15) . . ? 
O10 Si11 O11 109.81(16) . . ? 
O14 Si11 O22 110.47(14) . . ? 
O10 Si11 O22 109.39(15) . . ? 
O11 Si11 O22 107.87(15) . . ? 
O11 Si12 O20 109.89(15) . . ? 
O11 Si12 O12 108.74(17) . . ? 
O20 Si12 O12 109.61(15) . . ? 
O11 Si12 O24 109.92(14) . . ? 
O20 Si12 O24 107.39(15) . . ? 
O12 Si12 O24 111.28(15) . . ? 
O42 Si13 O27 111.15(16) . . ? 
O42 Si13 O41 108.70(16) . . ? 
O27 Si13 O41 110.56(17) . . ? 
O42 Si13 O21 109.52(14) . 2 ? 
O27 Si13 O21 108.28(14) . 2 ? 
O41 Si13 O21 108.59(14) . 2 ? 
O39 Si14 O32 108.76(16) . . ? 
O39 Si14 O27 110.39(16) . . ? 
O32 Si14 O27 109.69(17) . . ? 
O39 Si14 O28 110.02(17) . . ? 
O32 Si14 O28 109.97(14) . . ? 
O27 Si14 O28 108.02(14) . . ? 
O19 Si15 O20 110.41(16) 4_566 4_566 ? 
O19 Si15 O28 109.45(17) 4_566 . ? 
O20 Si15 O28 108.27(15) 4_566 . ? 
O19 Si15 O29 109.57(17) 4_566 . ? 
O20 Si15 O29 110.42(16) 4_566 . ? 
O28 Si15 O29 108.68(15) . . ? 
O29 Si16 O30 109.12(16) . . ? 
O29 Si16 O17 109.63(16) . 4_566 ? 
O30 Si16 O17 107.83(16) . 4_566 ? 
O29 Si16 O16 110.02(17) . 4_566 ? 
O30 Si16 O16 110.36(17) . 4_566 ? 
O17 Si16 O16 109.85(16) 4_566 4_566 ? 
O40 Si17 O31 109.25(14) . . ? 
O40 Si17 O30 109.19(16) . . ? 
O31 Si17 O30 110.31(15) . . ? 
O40 Si17 O47 110.87(14) . . ? 
O31 Si17 O47 108.47(14) . . ? 
O30 Si17 O47 108.73(14) . . ? 
O45 Si18 O44 109.99(18) . . ? 
O45 Si18 O32 110.16(15) . . ? 
O44 Si18 O32 110.13(15) . . ? 
O45 Si18 O31 109.77(14) . . ? 
O44 Si18 O31 106.96(13) . . ? 
O32 Si18 O31 109.78(16) . . ? 
O23 Si19 O33 110.36(15) . . ? 
O23 Si19 O22 110.52(14) . 2 ? 
O33 Si19 O22 108.08(15) . 2 ? 
O23 Si19 O43 107.22(14) . . ? 
O33 Si19 O43 110.25(15) . . ? 
O22 Si19 O43 110.42(14) 2 . ? 
O33 Si20 O39 109.78(16) . . ? 
O33 Si20 O34 108.83(15) . . ? 
O39 Si20 O34 110.32(17) . . ? 
O33 Si20 O38 110.16(17) . . ? 
O39 Si20 O38 108.85(16) . . ? 
O34 Si20 O38 108.88(15) . . ? 
O18 Si21 O25 107.03(14) 4_566 . ? 
O18 Si21 O34 108.84(14) 4_566 . ? 
O25 Si21 O34 111.90(14) . . ? 
O18 Si21 O35 109.88(16) 4_566 . ? 
O25 Si21 O35 110.69(13) . . ? 
O34 Si21 O35 108.47(16) . . ? 
O36 Si22 O15 109.75(17) . 4_566 ? 
O36 Si22 O35 108.56(17) . . ? 
O15 Si22 O35 109.84(16) 4_566 . ? 
O36 Si22 O26 109.69(15) . . ? 
O15 Si22 O26 108.09(13) 4_566 . ? 
O35 Si22 O26 110.89(13) . . ? 
O37 Si23 O36 110.54(17) . . ? 
O37 Si23 O48 108.32(15) . . ? 
O36 Si23 O48 108.80(16) . . ? 
O37 Si23 O40 109.01(15) . . ? 
O36 Si23 O40 109.41(16) . . ? 
O48 Si23 O40 110.76(14) . . ? 
O24 Si24 O38 108.79(15) . . ? 
O24 Si24 O37 109.09(14) . . ? 
O38 Si24 O37 109.08(17) . . ? 
O24 Si24 O46 107.93(16) . 4_666 ? 
O38 Si24 O46 110.93(16) . 4_666 ? 
O37 Si24 O46 110.97(16) . 4_666 ? 
Si2 O1 Si1 147.07(19) . . ? 
Si3 O2 Si2 148.30(18) . . ? 
Si4 O3 Si3 163.1(3) . . ? 
Si4 O4 Si5 150.47(17) . . ? 
Si6 O5 Si5 148.69(18) . . ? 
Si2 O6 Si6 162.8(2) . . ? 
Si8 O7 Si7 158.3(2) . . ? 
Si8 O8 Si9 153.4(2) . . ? 
Si10 O9 Si9 151.01(19) . . ? 
Si11 O10 Si10 156.6(2) . . ? 
Si12 O11 Si11 154.8(2) . . ? 
Si8 O12 Si12 171.0(2) . . ? 
Si8 O13 Si2 165.5(3) . . ? 
Si11 O14 Si5 162.1(2) . . ? 
Si1 O15 Si22 149.03(18) . 4_665 ? 
Si16 O16 Si1 176.2(2) 4_665 . ? 
Si16 O17 Si7 146.57(18) 4_665 . ? 
Si6 O18 Si21 142.72(19) . 4_665 ? 
Si15 O19 Si6 168.7(2) 4_665 . ? 
Si15 O20 Si12 144.00(19) 4_665 . ? 
Si5 O21 Si13 145.18(17) . 2_545 ? 
Si11 O22 Si19 151.16(19) . 2_545 ? 
Si19 O23 Si7 154.64(19) . . ? 
Si24 O24 Si12 149.31(19) . . ? 
Si9 O25 Si21 151.50(17) . . ? 
Si10 O26 Si22 146.91(16) . . ? 
Si14 O27 Si13 152.9(2) . . ? 
Si15 O28 Si14 150.56(17) . . ? 
Si16 O29 Si15 163.4(2) . . ? 
Si16 O30 Si17 158.9(2) . . ? 
Si17 O31 Si18 148.84(17) . . ? 
Si14 O32 Si18 157.9(2) . . ? 
Si20 O33 Si19 152.6(2) . . ? 
Si20 O34 Si21 148.75(17) . . ? 
Si22 O35 Si21 151.27(19) . . ? 
Si22 O36 Si23 162.1(2) . . ? 
Si23 O37 Si24 153.6(2) . . ? 
Si24 O38 Si20 156.3(2) . . ? 
Si14 O39 Si20 167.6(2) . . ? 
Si17 O40 Si23 163.01(18) . . ? 
Si10 O41 Si13 150.67(18) 4_666 . ? 
Si13 O42 Si4 159.0(2) . 4_666 ? 
Si4 O43 Si19 149.92(19) 4_666 . ? 
Si9 O44 Si18 149.01(17) 4_666 . ? 
Si18 O45 Si3 156.47(19) . 4_666 ? 
Si3 O46 Si24 153.8(2) . 4_565 ? 
Si1 O47 Si17 148.57(19) 2_545 . ? 
Si23 O48 Si7 149.1(2) . 2_545 ? 
  
_diffrn_measured_fraction_theta_max    0.940 
_diffrn_reflns_theta_full              27.61 
_diffrn_measured_fraction_theta_full   0.940 
_refine_diff_density_max    0.961 
_refine_diff_density_min   -0.548 
_refine_diff_density_rms    0.129 







  
data_f_pentane_twin_2h_2 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C5 O48 Si24' 
_chemical_formula_weight          1502 
  
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                    13.431(6) 
_cell_length_b                    20.148(8) 
_cell_length_c                    19.921(9) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.116(12) 
_cell_angle_gamma                 90.00 
_cell_volume                      5391(4) 
_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           0.07 
_exptl_crystal_size_min           0.04 
_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   0.8994 
_exptl_absorpt_correction_T_max   0.9755 
_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             63551 
_diffrn_reflns_av_R_equivalents   0.1466 
_diffrn_reflns_av_sigmaI/netI     0.1405 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        24 
_diffrn_reflns_limit_l_min        -26 
_diffrn_reflns_limit_l_max        26 
_diffrn_reflns_theta_min          1.83 
_diffrn_reflns_theta_max          28.75 
_reflns_number_total              12993 
_reflns_number_gt                 6408 
_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)+(0.0800P)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          12993 
_refine_ls_number_parameters      671 
_refine_ls_number_restraints      7 
_refine_ls_R_factor_all           0.1623 
_refine_ls_R_factor_gt            0.0594 
_refine_ls_wR_factor_ref          0.1791 
_refine_ls_wR_factor_gt           0.1484 
_refine_ls_goodness_of_fit_ref    0.975 
_refine_ls_restrained_S_all       0.977 
_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 
C301 C 0.167(2) 0.3061(11) 0.7427(17) 0.291(13) Uiso 1 1 d D A 1 
C302 C 0.129(2) 0.2410(13) 0.7668(16) 0.347(16) Uiso 1 1 d D A 1 
C303 C 0.146(2) 0.1763(12) 0.7367(17) 0.333(15) Uiso 1 1 d D A 1 
C304 C 0.1318(19) 0.1042(12) 0.7563(17) 0.288(12) Uiso 1 1 d D A 1 
C305 C 0.211(2) 0.0514(11) 0.746(2) 0.338(15) Uiso 1 1 d D A 1 
Si1 Si 0.32506(16) 0.42115(10) -0.05703(12) 0.0120(4) Uani 1 1 d . . . 
Si2 Si 0.17372(17) 0.31084(11) -0.03031(10) 0.0137(5) Uani 1 1 d . . . 
Si3 Si -0.04524(15) 0.27932(10) -0.06198(12) 0.0133(5) Uani 1 1 d . . . 
Si4 Si -0.03362(15) 0.12298(10) -0.06233(12) 0.0120(5) Uani 1 1 d . . . 
Si5 Si 0.17922(17) 0.07466(10) -0.02796(10) 0.0123(5) Uani 1 1 d . . . 
Si6 Si 0.31915(15) 0.19183(10) -0.05716(12) 0.0132(4) Uani 1 1 d . . . 
Si7 Si 0.32244(17) 0.42424(10) 0.17150(11) 0.0122(5) Uani 1 1 d . . . 
Si8 Si 0.17928(16) 0.31034(10) 0.12777(11) 0.0130(5) Uani 1 1 d . . . 
Si9 Si -0.03268(16) 0.27440(10) 0.17521(11) 0.0123(5) Uani 1 1 d . . . 
Si10 Si -0.03103(16) 0.12021(10) 0.17540(11) 0.0132(5) Uani 1 1 d . . . 
Si11 Si 0.17891(17) 0.07107(10) 0.13008(11) 0.0129(5) Uani 1 1 d . . . 
Si12 Si 0.31750(17) 0.18917(10) 0.16812(10) 0.0121(4) Uani 1 1 d . . . 
Si13 Si 0.33578(15) 0.42635(9) 0.55795(12) 0.0119(5) Uani 1 1 d . . . 
Si14 Si 0.19022(16) 0.31082(11) 0.52817(10) 0.0129(5) Uani 1 1 d . . . 
Si15 Si -0.02938(15) 0.27831(10) 0.56134(12) 0.0127(5) Uani 1 1 d . . . 
Si16 Si -0.03156(15) 0.12169(10) 0.56336(12) 0.0128(5) Uani 1 1 d . . . 
Si17 Si 0.18202(17) 0.07083(10) 0.52764(10) 0.0106(5) Uani 1 1 d . . . 
Si18 Si 0.32255(16) 0.18664(9) 0.56192(11) 0.0120(5) Uani 1 1 d . . . 
Si19 Si 0.31926(17) 0.42384(10) 0.32734(11) 0.0130(5) Uani 1 1 d . . . 
Si20 Si 0.17679(17) 0.31096(10) 0.37004(11) 0.0142(5) Uani 1 1 d . . . 
Si21 Si -0.03867(16) 0.27417(10) 0.33038(11) 0.0125(5) Uani 1 1 d . . . 
Si22 Si -0.03455(16) 0.11961(11) 0.32913(11) 0.0140(5) Uani 1 1 d . . . 
Si23 Si 0.17975(18) 0.07113(10) 0.36969(12) 0.0129(5) Uani 1 1 d . . . 
Si24 Si 0.30650(16) 0.19115(10) 0.32214(10) 0.0129(5) Uani 1 1 d . . . 
O1 O 0.2281(4) 0.3758(3) -0.0571(3) 0.0327(15) Uani 1 1 d . . . 
O2 O 0.0656(4) 0.3077(2) -0.0634(3) 0.0263(14) Uani 1 1 d . . . 
O3 O -0.0435(5) 0.2006(2) -0.0522(3) 0.0429(16) Uani 1 1 d . . . 
O4 O 0.0808(4) 0.1024(3) -0.0636(3) 0.0267(14) Uani 1 1 d . . . 
O5 O 0.2728(4) 0.1201(2) -0.0481(3) 0.0274(14) Uani 1 1 d . . . 
O6 O 0.2346(4) 0.2457(3) -0.0500(4) 0.0369(16) Uani 1 1 d . . . 
O7 O 0.2335(5) 0.3751(3) 0.1544(3) 0.0354(18) Uani 1 1 d . . . 
O8 O 0.0729(4) 0.3052(3) 0.1631(3) 0.0338(15) Uani 1 1 d . . . 
O9 O -0.0297(5) 0.1966(3) 0.1555(2) 0.0296(16) Uani 1 1 d . . . 
O10 O 0.0787(5) 0.0903(3) 0.1666(3) 0.0355(16) Uani 1 1 d . . . 
O11 O 0.2671(4) 0.1196(3) 0.1527(3) 0.0282(15) Uani 1 1 d . . . 
O12 O 0.2444(5) 0.2465(3) 0.1445(3) 0.0391(18) Uani 1 1 d . . . 
O13 O 0.1640(5) 0.3140(3) 0.0491(3) 0.0501(18) Uani 1 1 d . . . 
O14 O 0.1624(4) 0.0771(3) 0.0515(3) 0.0290(13) Uani 1 1 d . . . 
O15 O 0.3820(4) 0.4147(3) -0.1259(3) 0.0323(16) Uani 1 1 d . . . 
O16 O 0.3959(5) 0.3982(3) 0.0032(3) 0.0388(17) Uani 1 1 d . . . 
O17 O 0.4200(4) 0.4015(3) 0.1320(3) 0.0242(14) Uani 1 1 d . . . 
O18 O 0.3684(4) 0.1961(3) -0.1294(3) 0.0254(13) Uani 1 1 d . . . 
O19 O 0.4048(4) 0.2033(3) -0.0019(3) 0.0356(16) Uani 1 1 d . . . 
O20 O 0.4202(4) 0.1956(3) 0.1283(3) 0.0275(14) Uani 1 1 d . . . 
O21 O 0.2033(4) 0.0010(2) -0.0530(3) 0.0218(13) Uani 1 1 d . . . 
O22 O 0.2100(4) -0.0028(3) 0.1507(3) 0.0265(15) Uani 1 1 d . . . 
O23 O 0.3468(3) 0.4220(2) 0.2494(3) 0.0309(11) Uani 1 1 d . . . 
O24 O 0.3425(3) 0.1951(2) 0.2464(3) 0.0254(11) Uani 1 1 d . . . 
O25 O -0.0604(3) 0.28410(19) 0.2518(3) 0.0216(10) Uani 1 1 d . . . 
O26 O -0.0638(3) 0.11119(18) 0.2516(3) 0.0211(10) Uani 1 1 d . . . 
O27 O 0.2418(4) 0.3770(3) 0.5541(4) 0.0360(16) Uani 1 1 d . . . 
O28 O 0.0780(4) 0.3114(2) 0.5544(3) 0.0249(13) Uani 1 1 d . . . 
O29 O -0.0169(4) 0.1992(2) 0.5643(3) 0.0395(16) Uani 1 1 d . . . 
O30 O 0.0731(4) 0.0863(3) 0.5550(3) 0.0316(14) Uani 1 1 d . . . 
O31 O 0.2623(4) 0.1187(3) 0.5614(3) 0.0240(13) Uani 1 1 d . . . 
O32 O 0.2471(4) 0.2483(3) 0.5585(3) 0.0295(14) Uani 1 1 d . . . 
O33 O 0.2257(4) 0.3771(3) 0.3419(3) 0.0280(15) Uani 1 1 d . . . 
O34 O 0.0600(4) 0.3119(2) 0.3522(3) 0.0249(14) Uani 1 1 d . . . 
O35 O -0.0259(5) 0.1963(2) 0.3476(3) 0.0310(16) Uani 1 1 d . . . 
O36 O 0.0698(5) 0.0860(3) 0.3435(3) 0.0406(18) Uani 1 1 d . . . 
O37 O 0.2567(5) 0.1204(3) 0.3349(3) 0.0384(17) Uani 1 1 d . . . 
O38 O 0.2261(5) 0.2474(3) 0.3351(3) 0.0384(16) Uani 1 1 d . . . 
O39 O 0.1932(4) 0.3063(3) 0.4488(3) 0.0446(16) Uani 1 1 d . . . 
O40 O 0.1841(4) 0.0810(3) 0.4490(3) 0.0360(15) Uani 1 1 d . . . 
O41 O 0.3902(4) 0.4177(3) 0.6290(3) 0.0304(15) Uani 1 1 d . . . 
O42 O 0.4131(4) 0.4123(3) 0.4994(3) 0.0297(14) Uani 1 1 d . . . 
O43 O 0.4151(4) 0.3989(3) 0.3686(3) 0.0294(15) Uani 1 1 d . . . 
O44 O 0.3857(4) 0.1896(3) 0.6298(3) 0.0238(13) Uani 1 1 d . . . 
O45 O 0.3947(4) 0.1887(3) 0.4989(3) 0.0302(14) Uani 1 1 d . . . 
O46 O -0.0976(4) 0.2985(3) -0.1305(3) 0.0349(16) Uani 1 1 d . . . 
O47 O 0.2099(4) -0.0042(2) 0.5458(3) 0.0237(14) Uani 1 1 d . . . 
O48 O 0.2091(4) -0.0026(3) 0.3507(3) 0.0280(15) 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 1.487(17) . ? 
C302 C303 1.454(18) . ? 
C303 C304 1.518(17) . ? 
C304 C305 1.516(17) . ? 
Si1 O15 1.578(6) . ? 
Si1 O1 1.590(5) . ? 
Si1 O47 1.591(5) 2 ? 
Si1 O16 1.598(6) . ? 
Si2 O13 1.588(6) . ? 
Si2 O1 1.592(6) . ? 
Si2 O2 1.595(5) . ? 
Si2 O6 1.596(6) . ? 
Si3 O46 1.582(6) . ? 
Si3 O45 1.594(6) 4_565 ? 
Si3 O2 1.595(5) . ? 
Si3 O3 1.599(5) . ? 
Si4 O3 1.582(5) . ? 
Si4 O42 1.591(6) 4_565 ? 
Si4 O4 1.592(5) . ? 
Si4 O43 1.599(6) 4_565 ? 
Si5 O21 1.598(5) . ? 
Si5 O4 1.600(5) . ? 
Si5 O14 1.600(6) . ? 
Si5 O5 1.606(5) . ? 
Si6 O6 1.578(5) . ? 
Si6 O5 1.585(5) . ? 
Si6 O18 1.587(6) . ? 
Si6 O19 1.607(6) . ? 
Si7 O23 1.586(7) . ? 
Si7 O7 1.588(6) . ? 
Si7 O48 1.596(6) 2 ? 
Si7 O17 1.597(6) . ? 
Si8 O13 1.582(6) . ? 
Si8 O7 1.586(6) . ? 
Si8 O12 1.591(6) . ? 
Si8 O8 1.597(6) . ? 
Si9 O8 1.567(6) . ? 
Si9 O25 1.583(6) . ? 
Si9 O44 1.595(6) 4_565 ? 
Si9 O9 1.618(5) . ? 
Si10 O9 1.589(5) . ? 
Si10 O26 1.592(6) . ? 
Si10 O41 1.598(6) 4_565 ? 
Si10 O10 1.602(6) . ? 
Si11 O10 1.579(6) . ? 
Si11 O14 1.585(6) . ? 
Si11 O22 1.599(6) . ? 
Si11 O11 1.600(6) . ? 
Si12 O12 1.586(6) . ? 
Si12 O11 1.586(6) . ? 
Si12 O20 1.597(6) . ? 
Si12 O24 1.600(6) . ? 
Si13 O42 1.589(6) . ? 
Si13 O21 1.597(5) 2 ? 
Si13 O41 1.601(6) . ? 
Si13 O27 1.608(5) . ? 
Si14 O39 1.584(6) . ? 
Si14 O27 1.589(5) . ? 
Si14 O32 1.591(5) . ? 
Si14 O28 1.596(5) . ? 
Si15 O19 1.581(6) 4_566 ? 
Si15 O20 1.587(6) 4_566 ? 
Si15 O28 1.595(5) . ? 
Si15 O29 1.604(5) . ? 
Si16 O29 1.574(5) . ? 
Si16 O30 1.585(5) . ? 
Si16 O17 1.586(6) 4_566 ? 
Si16 O16 1.594(6) 4_566 ? 
Si17 O40 1.579(6) . ? 
Si17 O30 1.593(6) . ? 
Si17 O31 1.595(5) . ? 
Si17 O47 1.599(5) . ? 
Si18 O45 1.588(6) . ? 
Si18 O31 1.590(5) . ? 
Si18 O44 1.595(6) . ? 
Si18 O32 1.605(5) . ? 
Si19 O22 1.591(6) 2 ? 
Si19 O23 1.597(7) . ? 
Si19 O33 1.597(6) . ? 
Si19 O43 1.606(6) . ? 
Si20 O39 1.587(6) . ? 
Si20 O33 1.589(6) . ? 
Si20 O38 1.601(6) . ? 
Si20 O34 1.608(6) . ? 
Si21 O34 1.588(5) . ? 
Si21 O18 1.601(6) 4_566 ? 
Si21 O25 1.605(6) . ? 
Si21 O35 1.615(5) . ? 
Si22 O36 1.583(6) . ? 
Si22 O35 1.593(5) . ? 
Si22 O15 1.593(6) 4_566 ? 
Si22 O26 1.602(6) . ? 
Si23 O48 1.582(6) . ? 
Si23 O37 1.593(6) . ? 
Si23 O36 1.593(6) . ? 
Si23 O40 1.594(6) . ? 
Si24 O24 1.587(6) . ? 
Si24 O38 1.588(6) . ? 
Si24 O37 1.595(6) . ? 
Si24 O46 1.609(6) 4_666 ? 
O15 Si22 1.593(6) 4_665 ? 
O16 Si16 1.594(6) 4_665 ? 
O17 Si16 1.586(6) 4_665 ? 
O18 Si21 1.601(6) 4_665 ? 
O19 Si15 1.581(6) 4_665 ? 
O20 Si15 1.587(6) 4_665 ? 
O21 Si13 1.597(5) 2_545 ? 
O22 Si19 1.591(6) 2_545 ? 
O41 Si10 1.598(6) 4_666 ? 
O42 Si4 1.591(6) 4_666 ? 
O43 Si4 1.599(6) 4_666 ? 
O44 Si9 1.595(6) 4_666 ? 
O45 Si3 1.595(6) 4_666 ? 
O46 Si24 1.609(6) 4_565 ? 
O47 Si1 1.591(5) 2_545 ? 
O48 Si7 1.596(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 
C303 C302 C301 127(3) . . ? 
C302 C303 C304 137(3) . . ? 
C305 C304 C303 123(2) . . ? 
O15 Si1 O1 110.5(4) . . ? 
O15 Si1 O47 110.1(3) . 2 ? 
O1 Si1 O47 107.5(3) . 2 ? 
O15 Si1 O16 109.9(3) . . ? 
O1 Si1 O16 108.7(3) . . ? 
O47 Si1 O16 110.1(3) 2 . ? 
O13 Si2 O1 109.9(4) . . ? 
O13 Si2 O2 109.6(3) . . ? 
O1 Si2 O2 108.2(3) . . ? 
O13 Si2 O6 108.7(4) . . ? 
O1 Si2 O6 111.0(3) . . ? 
O2 Si2 O6 109.4(3) . . ? 
O46 Si3 O45 109.4(3) . 4_565 ? 
O46 Si3 O2 108.1(3) . . ? 
O45 Si3 O2 110.0(3) 4_565 . ? 
O46 Si3 O3 110.8(4) . . ? 
O45 Si3 O3 108.4(4) 4_565 . ? 
O2 Si3 O3 110.2(3) . . ? 
O3 Si4 O42 107.7(3) . 4_565 ? 
O3 Si4 O4 109.9(3) . . ? 
O42 Si4 O4 109.4(3) 4_565 . ? 
O3 Si4 O43 110.2(3) . 4_565 ? 
O42 Si4 O43 110.3(3) 4_565 4_565 ? 
O4 Si4 O43 109.2(3) . 4_565 ? 
O21 Si5 O4 110.7(3) . . ? 
O21 Si5 O14 111.5(3) . . ? 
O4 Si5 O14 108.1(3) . . ? 
O21 Si5 O5 106.9(3) . . ? 
O4 Si5 O5 109.6(3) . . ? 
O14 Si5 O5 110.0(3) . . ? 
O6 Si6 O5 109.5(3) . . ? 
O6 Si6 O18 110.3(4) . . ? 
O5 Si6 O18 108.5(3) . . ? 
O6 Si6 O19 110.7(4) . . ? 
O5 Si6 O19 109.5(3) . . ? 
O18 Si6 O19 108.3(3) . . ? 
O23 Si7 O7 110.2(3) . . ? 
O23 Si7 O48 110.6(3) . 2 ? 
O7 Si7 O48 108.5(3) . 2 ? 
O23 Si7 O17 107.8(3) . . ? 
O7 Si7 O17 109.5(3) . . ? 
O48 Si7 O17 110.3(3) 2 . ? 
O13 Si8 O7 110.6(3) . . ? 
O13 Si8 O12 108.4(3) . . ? 
O7 Si8 O12 110.1(4) . . ? 
O13 Si8 O8 109.0(3) . . ? 
O7 Si8 O8 108.4(3) . . ? 
O12 Si8 O8 110.3(3) . . ? 
O8 Si9 O25 108.3(3) . . ? 
O8 Si9 O44 110.7(3) . 4_565 ? 
O25 Si9 O44 109.2(3) . 4_565 ? 
O8 Si9 O9 108.9(3) . . ? 
O25 Si9 O9 111.1(3) . . ? 
O44 Si9 O9 108.7(3) 4_565 . ? 
O9 Si10 O26 110.6(3) . . ? 
O9 Si10 O41 109.0(3) . 4_565 ? 
O26 Si10 O41 108.3(3) . 4_565 ? 
O9 Si10 O10 109.0(3) . . ? 
O26 Si10 O10 108.5(3) . . ? 
O41 Si10 O10 111.4(4) 4_565 . ? 
O10 Si11 O14 108.5(3) . . ? 
O10 Si11 O22 109.4(3) . . ? 
O14 Si11 O22 111.1(3) . . ? 
O10 Si11 O11 110.6(3) . . ? 
O14 Si11 O11 109.5(3) . . ? 
O22 Si11 O11 107.7(3) . . ? 
O12 Si12 O11 108.8(3) . . ? 
O12 Si12 O20 109.2(3) . . ? 
O11 Si12 O20 110.1(3) . . ? 
O12 Si12 O24 111.3(3) . . ? 
O11 Si12 O24 110.1(3) . . ? 
O20 Si12 O24 107.4(3) . . ? 
O42 Si13 O21 109.7(3) . 2 ? 
O42 Si13 O41 109.4(3) . . ? 
O21 Si13 O41 107.9(3) 2 . ? 
O42 Si13 O27 111.6(3) . . ? 
O21 Si13 O27 108.8(3) 2 . ? 
O41 Si13 O27 109.4(4) . . ? 
O39 Si14 O27 111.2(4) . . ? 
O39 Si14 O32 108.7(3) . . ? 
O27 Si14 O32 109.4(3) . . ? 
O39 Si14 O28 110.6(3) . . ? 
O27 Si14 O28 107.4(3) . . ? 
O32 Si14 O28 109.5(3) . . ? 
O19 Si15 O20 110.6(3) 4_566 4_566 ? 
O19 Si15 O28 109.7(4) 4_566 . ? 
O20 Si15 O28 108.8(3) 4_566 . ? 
O19 Si15 O29 108.7(3) 4_566 . ? 
O20 Si15 O29 110.1(3) 4_566 . ? 
O28 Si15 O29 108.9(3) . . ? 
O29 Si16 O30 109.7(3) . . ? 
O29 Si16 O17 109.4(3) . 4_566 ? 
O30 Si16 O17 108.9(3) . 4_566 ? 
O29 Si16 O16 109.6(3) . 4_566 ? 
O30 Si16 O16 110.4(4) . 4_566 ? 
O17 Si16 O16 108.8(3) 4_566 4_566 ? 
O40 Si17 O30 109.4(3) . . ? 
O40 Si17 O31 109.1(3) . . ? 
O30 Si17 O31 111.0(3) . . ? 
O40 Si17 O47 110.1(3) . . ? 
O30 Si17 O47 108.8(3) . . ? 
O31 Si17 O47 108.6(3) . . ? 
O45 Si18 O31 109.2(3) . . ? 
O45 Si18 O44 110.1(3) . . ? 
O31 Si18 O44 107.9(3) . . ? 
O45 Si18 O32 109.4(3) . . ? 
O31 Si18 O32 110.2(3) . . ? 
O44 Si18 O32 110.0(3) . . ? 
O22 Si19 O23 110.3(3) 2 . ? 
O22 Si19 O33 107.6(3) 2 . ? 
O23 Si19 O33 110.3(3) . . ? 
O22 Si19 O43 110.4(3) 2 . ? 
O23 Si19 O43 107.6(3) . . ? 
O33 Si19 O43 110.6(3) . . ? 
O39 Si20 O33 110.0(3) . . ? 
O39 Si20 O38 109.0(3) . . ? 
O33 Si20 O38 110.2(3) . . ? 
O39 Si20 O34 110.7(3) . . ? 
O33 Si20 O34 108.4(3) . . ? 
O38 Si20 O34 108.5(3) . . ? 
O34 Si21 O18 109.6(3) . 4_566 ? 
O34 Si21 O25 110.9(3) . . ? 
O18 Si21 O25 107.6(3) 4_566 . ? 
O34 Si21 O35 108.6(3) . . ? 
O18 Si21 O35 109.8(3) 4_566 . ? 
O25 Si21 O35 110.3(3) . . ? 
O36 Si22 O35 108.0(3) . . ? 
O36 Si22 O15 109.7(3) . 4_566 ? 
O35 Si22 O15 110.0(3) . 4_566 ? 
O36 Si22 O26 110.2(3) . . ? 
O35 Si22 O26 110.0(3) . . ? 
O15 Si22 O26 108.9(3) 4_566 . ? 
O48 Si23 O37 108.6(3) . . ? 
O48 Si23 O36 109.2(3) . . ? 
O37 Si23 O36 110.0(4) . . ? 
O48 Si23 O40 110.3(3) . . ? 
O37 Si23 O40 109.3(3) . . ? 
O36 Si23 O40 109.5(3) . . ? 
O24 Si24 O38 109.1(3) . . ? 
O24 Si24 O37 109.0(3) . . ? 
O38 Si24 O37 109.1(4) . . ? 
O24 Si24 O46 107.8(3) . 4_666 ? 
O38 Si24 O46 110.9(3) . 4_666 ? 
O37 Si24 O46 110.9(3) . 4_666 ? 
Si1 O1 Si2 148.0(4) . . ? 
Si2 O2 Si3 148.9(4) . . ? 
Si4 O3 Si3 165.1(5) . . ? 
Si4 O4 Si5 151.7(4) . . ? 
Si6 O5 Si5 148.9(4) . . ? 
Si6 O6 Si2 163.2(5) . . ? 
Si8 O7 Si7 158.3(5) . . ? 
Si9 O8 Si8 154.6(4) . . ? 
Si10 O9 Si9 151.3(4) . . ? 
Si11 O10 Si10 158.1(4) . . ? 
Si12 O11 Si11 155.5(4) . . ? 
Si12 O12 Si8 172.2(5) . . ? 
Si8 O13 Si2 166.9(5) . . ? 
Si11 O14 Si5 162.7(4) . . ? 
Si1 O15 Si22 150.2(4) . 4_665 ? 
Si16 O16 Si1 177.7(5) 4_665 . ? 
Si16 O17 Si7 148.0(4) 4_665 . ? 
Si6 O18 Si21 143.3(4) . 4_665 ? 
Si15 O19 Si6 167.8(5) 4_665 . ? 
Si15 O20 Si12 144.5(4) 4_665 . ? 
Si13 O21 Si5 145.8(4) 2_545 . ? 
Si19 O22 Si11 150.5(4) 2_545 . ? 
Si7 O23 Si19 154.5(3) . . ? 
Si24 O24 Si12 149.3(3) . . ? 
Si9 O25 Si21 151.9(3) . . ? 
Si10 O26 Si22 147.1(3) . . ? 
Si14 O27 Si13 151.2(4) . . ? 
Si15 O28 Si14 151.6(4) . . ? 
Si16 O29 Si15 166.6(4) . . ? 
Si16 O30 Si17 159.8(4) . . ? 
Si18 O31 Si17 150.1(4) . . ? 
Si14 O32 Si18 158.7(4) . . ? 
Si20 O33 Si19 152.2(4) . . ? 
Si21 O34 Si20 150.2(4) . . ? 
Si22 O35 Si21 152.4(4) . . ? 
Si22 O36 Si23 163.6(5) . . ? 
Si23 O37 Si24 154.0(4) . . ? 
Si24 O38 Si20 157.5(5) . . ? 
Si14 O39 Si20 168.4(4) . . ? 
Si17 O40 Si23 165.0(4) . . ? 
Si10 O41 Si13 149.8(4) 4_666 . ? 
Si13 O42 Si4 160.5(4) . 4_666 ? 
Si4 O43 Si19 150.5(4) 4_666 . ? 
Si9 O44 Si18 149.5(4) 4_666 . ? 
Si18 O45 Si3 157.3(4) . 4_666 ? 
Si3 O46 Si24 153.1(4) . 4_565 ? 
Si1 O47 Si17 148.9(4) 2_545 . ? 
Si23 O48 Si7 150.1(4) . 2_545 ? 
  
_diffrn_measured_fraction_theta_max    0.928 
_diffrn_reflns_theta_full              28.75 
_diffrn_measured_fraction_theta_full   0.928 
_refine_diff_density_max    1.047 
_refine_diff_density_min   -0.608 
_refine_diff_density_rms    0.174 



  
data_f_t2butene_twin_02atm_1h 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C4.5 H0 O48 Si24' 
_chemical_formula_weight          1497
  
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                    13.448(9) 
_cell_length_b                    20.156(14) 
_cell_length_c                    19.971(14) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  89.962(7) 
_cell_angle_gamma                 90.00 
_cell_volume                      5413(6) 
_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           0.14 
_exptl_crystal_size_mid           0.09 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.838 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3008 
_exptl_absorpt_coefficient_mu     0.669 
_exptl_absorpt_correction_type    Analytical 
_exptl_absorpt_correction_T_min   0.9122 
_exptl_absorpt_correction_T_max   0.9572 
_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             63116 
_diffrn_reflns_av_R_equivalents   0.0844 
_diffrn_reflns_av_sigmaI/netI     0.1133 
_diffrn_reflns_limit_h_min        -17 
_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        26 
_diffrn_reflns_theta_min          1.01 
_diffrn_reflns_theta_max          28.60 
_reflns_number_total              13015 
_reflns_number_gt                 5390 
_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)+(0.0661P)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          13015 
_refine_ls_number_parameters      666 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1332 
_refine_ls_R_factor_gt            0.0513 
_refine_ls_wR_factor_ref          0.1649 
_refine_ls_wR_factor_gt           0.1423 
_refine_ls_goodness_of_fit_ref    0.887 
_refine_ls_restrained_S_all       0.887 
_refine_ls_shift/su_max           0.067 
_refine_ls_shift/su_mean          0.009 
  
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 0.6369(10) 0.2287(8) 0.2413(11) 0.187(10) Uiso 0.811(12) 1 d PG A 1 
C302 C 0.6482(7) 0.2964(7) 0.2726(8) 0.169(11) Uiso 0.811(12) 1 d PG A 1 
C303 C 0.6438(8) 0.3536(8) 0.2379(8) 0.162(9) Uiso 0.811(12) 1 d PG A 1 
C304 C 0.6551(9) 0.4213(7) 0.2693(10) 0.264(16) Uiso 0.811(12) 1 d PG A 1 
C101 C 0.9689(19) 0.4941(15) 0.5520(8) 0.13(2) Uiso 0.322(8) 1 d PG . 2 
C102 C 1.0205(14) 0.4936(11) 0.4850(9) 0.043(9) Uiso 0.322(8) 1 d PG . 2 
C103 C 0.9727(11) 0.4986(9) 0.4259(8) 0.060(10) Uiso 0.322(8) 1 d PG . 2 
C104 C 1.0244(11) 0.4980(9) 0.3589(9) 0.079(13) Uiso 0.322(8) 1 d PG . 2 
Si1 Si 0.3325(2) 0.42235(15) -0.0575(2) 0.0168(7) Uani 1 1 d . . . 
Si2 Si 0.1845(3) 0.30871(17) -0.02991(15) 0.0187(7) Uani 1 1 d . . . 
Si3 Si -0.0357(2) 0.27937(16) -0.0624(2) 0.0192(8) Uani 1 1 d . . . 
Si4 Si -0.0295(2) 0.12229(16) -0.06338(19) 0.0170(8) Uani 1 1 d . . . 
Si5 Si 0.1825(2) 0.07349(16) -0.02837(16) 0.0158(8) Uani 1 1 d . . . 
Si6 Si 0.3268(2) 0.18805(16) -0.05822(19) 0.0182(7) Uani 1 1 d . . . 
Si7 Si 0.3251(3) 0.42346(17) 0.17153(18) 0.0172(8) Uani 1 1 d . . . 
Si8 Si 0.1847(2) 0.30764(17) 0.12811(18) 0.0177(7) Uani 1 1 d . . . 
Si9 Si -0.0297(2) 0.27341(18) 0.17338(18) 0.0176(8) Uani 1 1 d . . . 
Si10 Si -0.0275(3) 0.11945(18) 0.17431(18) 0.0194(8) Uani 1 1 d . . . 
Si11 Si 0.1833(3) 0.07058(15) 0.12921(18) 0.0163(7) Uani 1 1 d . . . 
Si12 Si 0.3207(3) 0.18681(17) 0.17038(17) 0.0177(7) Uani 1 1 d . . . 
Si13 Si 0.3390(2) 0.42415(15) 0.5571(2) 0.0165(7) Uani 1 1 d . . . 
Si14 Si 0.1928(2) 0.30870(18) 0.52867(16) 0.0186(8) Uani 1 1 d . . . 
Si15 Si -0.0282(2) 0.27986(16) 0.5609(2) 0.0172(7) Uani 1 1 d . . . 
Si16 Si -0.0268(2) 0.12332(16) 0.56394(18) 0.0160(7) Uani 1 1 d . . . 
Si17 Si 0.1866(2) 0.07062(16) 0.52852(16) 0.0141(7) Uani 1 1 d . . . 
Si18 Si 0.3271(2) 0.18556(16) 0.56110(19) 0.0185(7) Uani 1 1 d . . . 
Si19 Si 0.3232(3) 0.42285(17) 0.32755(18) 0.0173(8) Uani 1 1 d . . . 
Si20 Si 0.1827(2) 0.30872(17) 0.37010(17) 0.0176(7) Uani 1 1 d . . . 
Si21 Si -0.0329(2) 0.27393(17) 0.32890(18) 0.0182(8) Uani 1 1 d . . . 
Si22 Si -0.0296(3) 0.11901(18) 0.32809(18) 0.0176(8) Uani 1 1 d . . . 
Si23 Si 0.1835(3) 0.06997(16) 0.36997(19) 0.0179(8) Uani 1 1 d . . . 
Si24 Si 0.3151(3) 0.18794(17) 0.32470(16) 0.0180(7) Uani 1 1 d . . . 
O1 O 0.2390(6) 0.3736(4) -0.0572(6) 0.045(3) Uani 1 1 d . . . 
O2 O 0.0744(6) 0.3077(4) -0.0627(5) 0.036(2) Uani 1 1 d . . . 
O3 O -0.0364(7) 0.2008(4) -0.0578(6) 0.051(3) Uani 1 1 d . . . 
O4 O 0.0846(5) 0.0988(4) -0.0629(5) 0.033(2) Uani 1 1 d . . . 
O5 O 0.2775(5) 0.1157(3) -0.0539(6) 0.032(2) Uani 1 1 d . . . 
O6 O 0.2426(6) 0.2433(4) -0.0478(6) 0.050(3) Uani 1 1 d . . . 
O7 O 0.2395(7) 0.3727(4) 0.1574(5) 0.040(3) Uani 1 1 d . . . 
O8 O 0.0754(6) 0.3048(4) 0.1607(4) 0.040(2) Uani 1 1 d . . . 
O9 O -0.0265(7) 0.1951(4) 0.1546(4) 0.032(2) Uani 1 1 d . . . 
O10 O 0.0802(6) 0.0891(5) 0.1649(5) 0.040(3) Uani 1 1 d . . . 
O11 O 0.2728(6) 0.1166(4) 0.1541(5) 0.030(2) Uani 1 1 d . . . 
O12 O 0.2494(6) 0.2436(4) 0.1481(5) 0.048(3) Uani 1 1 d . . . 
O13 O 0.1812(8) 0.3113(5) 0.0499(5) 0.068(3) Uani 1 1 d . . . 
O14 O 0.1686(6) 0.0796(4) 0.0508(5) 0.035(2) Uani 1 1 d . . . 
O15 O 0.3909(7) 0.4180(4) -0.1278(4) 0.037(2) Uani 1 1 d . . . 
O16 O 0.4067(7) 0.4041(5) 0.0005(5) 0.048(3) Uani 1 1 d . . . 
O17 O 0.4225(6) 0.3993(5) 0.1341(5) 0.034(2) Uani 1 1 d . . . 
O18 O 0.3761(5) 0.1952(4) -0.1294(4) 0.030(2) Uani 1 1 d . . . 
O19 O 0.4102(7) 0.1947(5) -0.0022(4) 0.040(2) Uani 1 1 d . . . 
O20 O 0.4224(6) 0.1951(4) 0.1287(4) 0.033(2) Uani 1 1 d . . . 
O21 O 0.2039(6) -0.0031(4) -0.0512(5) 0.032(2) Uani 1 1 d . . . 
O22 O 0.2086(6) -0.0045(4) 0.1477(5) 0.034(2) Uani 1 1 d . . . 
O23 O 0.3492(3) 0.4238(2) 0.2503(6) 0.0345(11) Uani 1 1 d . . . 
O24 O 0.3472(3) 0.1929(2) 0.2492(5) 0.0301(11) Uani 1 1 d . . . 
O25 O -0.0544(3) 0.2832(2) 0.2494(5) 0.0284(11) Uani 1 1 d . . . 
O26 O -0.0609(3) 0.10999(19) 0.2493(5) 0.0246(10) Uani 1 1 d . . . 
O27 O 0.2487(6) 0.3723(4) 0.5562(6) 0.037(2) Uani 1 1 d . . . 
O28 O 0.0809(5) 0.3097(4) 0.5557(5) 0.0293(19) Uani 1 1 d . . . 
O29 O -0.0236(7) 0.2015(4) 0.5595(6) 0.052(3) Uani 1 1 d . . . 
O30 O 0.0818(6) 0.0937(5) 0.5614(6) 0.045(3) Uani 1 1 d . . . 
O31 O 0.2722(6) 0.1159(4) 0.5573(5) 0.030(2) Uani 1 1 d . . . 
O32 O 0.2467(6) 0.2442(4) 0.5581(5) 0.035(2) Uani 1 1 d . . . 
O33 O 0.2309(6) 0.3726(4) 0.3407(5) 0.038(3) Uani 1 1 d . . . 
O34 O 0.0673(6) 0.3088(4) 0.3513(4) 0.033(2) Uani 1 1 d . . . 
O35 O -0.0267(7) 0.1973(4) 0.3479(4) 0.040(3) Uani 1 1 d . . . 
O36 O 0.0789(7) 0.0882(5) 0.3395(5) 0.052(3) Uani 1 1 d . . . 
O37 O 0.2652(7) 0.1181(5) 0.3368(5) 0.042(3) Uani 1 1 d . . . 
O38 O 0.2302(6) 0.2433(4) 0.3390(5) 0.042(2) Uani 1 1 d . . . 
O39 O 0.1916(7) 0.3083(5) 0.4499(5) 0.060(3) Uani 1 1 d . . . 
O40 O 0.1817(6) 0.0798(4) 0.4495(4) 0.040(2) Uani 1 1 d . . . 
O41 O 0.3929(7) 0.4190(4) 0.6270(5) 0.037(3) Uani 1 1 d . . . 
O42 O 0.4155(7) 0.4099(5) 0.4964(4) 0.036(2) Uani 1 1 d . . . 
O43 O 0.4221(6) 0.4005(4) 0.3686(4) 0.032(2) Uani 1 1 d . . . 
O44 O 0.3885(6) 0.1891(4) 0.6306(4) 0.031(2) Uani 1 1 d . . . 
O45 O 0.4035(7) 0.1914(5) 0.4989(4) 0.042(3) Uani 1 1 d . . . 
O46 O -0.0871(6) 0.3015(5) -0.1310(4) 0.045(3) Uani 1 1 d . . . 
O47 O 0.2082(5) -0.0034(3) 0.5465(5) 0.0224(19) Uani 1 1 d . . . 
O48 O 0.2117(6) -0.0057(4) 0.3528(5) 0.029(2) 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 1.5081 . ? 
C302 C303 1.3465 . ? 
C303 C304 1.5080 . ? 
C101 C102 0.79(4) 3_766 ? 
C101 C103 0.91(4) 3_766 ? 
C101 C102 1.5072 . ? 
C101 C104 1.79(3) 3_766 ? 
C102 C101 0.79(4) 3_766 ? 
C102 C102 0.86(4) 3_766 ? 
C102 C103 1.3483 . ? 
C102 C103 1.79(3) 3_766 ? 
C103 C101 0.91(3) 3_766 ? 
C103 C104 1.5071 . ? 
C103 C102 1.79(3) 3_766 ? 
C104 C101 1.79(3) 3_766 ? 
Si1 O16 1.574(9) . ? 
Si1 O1 1.596(8) . ? 
Si1 O47 1.609(7) 2 ? 
Si1 O15 1.610(9) . ? 
Si2 O6 1.575(8) . ? 
Si2 O1 1.595(9) . ? 
Si2 O13 1.596(10) . ? 
Si2 O2 1.619(9) . ? 
Si3 O45 1.585(9) 4_565 ? 
Si3 O3 1.586(8) . ? 
Si3 O2 1.587(9) . ? 
Si3 O46 1.600(9) . ? 
Si4 O42 1.546(9) 4_565 ? 
Si4 O43 1.575(9) 4_565 ? 
Si4 O3 1.589(8) . ? 
Si4 O4 1.607(8) . ? 
Si5 O4 1.571(8) . ? 
Si5 O14 1.597(10) . ? 
Si5 O5 1.618(8) . ? 
Si5 O21 1.634(8) . ? 
Si6 O18 1.575(8) . ? 
Si6 O19 1.591(9) . ? 
Si6 O6 1.601(8) . ? 
Si6 O5 1.603(7) . ? 
Si7 O7 1.566(9) . ? 
Si7 O17 1.585(9) . ? 
Si7 O48 1.587(8) 2 ? 
Si7 O23 1.607(11) . ? 
Si8 O13 1.564(10) . ? 
Si8 O12 1.607(8) . ? 
Si8 O8 1.608(9) . ? 
Si8 O7 1.614(9) . ? 
Si9 O25 1.566(10) . ? 
Si9 O8 1.569(9) . ? 
Si9 O44 1.586(9) 4_565 ? 
Si9 O9 1.623(9) . ? 
Si10 O26 1.574(11) . ? 
Si10 O9 1.575(9) . ? 
Si10 O10 1.583(9) . ? 
Si10 O41 1.625(8) 4_565 ? 
Si11 O14 1.589(10) . ? 
Si11 O22 1.594(9) . ? 
Si11 O11 1.600(9) . ? 
Si11 O10 1.602(9) . ? 
Si12 O12 1.559(8) . ? 
Si12 O11 1.588(8) . ? 
Si12 O20 1.609(9) . ? 
Si12 O24 1.619(10) . ? 
Si13 O41 1.577(10) . ? 
Si13 O21 1.581(8) 2 ? 
Si13 O27 1.602(7) . ? 
Si13 O42 1.616(10) . ? 
Si14 O39 1.574(9) . ? 
Si14 O27 1.585(8) . ? 
Si14 O28 1.598(8) . ? 
Si14 O32 1.601(8) . ? 
Si15 O29 1.580(8) . ? 
Si15 O20 1.590(9) 4_566 ? 
Si15 O28 1.590(8) . ? 
Si15 O19 1.593(9) 4_566 ? 
Si16 O30 1.579(8) . ? 
Si16 O29 1.580(8) . ? 
Si16 O17 1.622(9) 4_566 ? 
Si16 O16 1.646(9) 4_566 ? 
Si17 O47 1.562(7) . ? 
Si17 O31 1.578(8) . ? 
Si17 O40 1.590(9) . ? 
Si17 O30 1.623(9) . ? 
Si18 O31 1.588(8) . ? 
Si18 O32 1.603(8) . ? 
Si18 O45 1.616(9) . ? 
Si18 O44 1.617(9) . ? 
Si19 O23 1.581(11) . ? 
Si19 O22 1.604(9) 2 ? 
Si19 O33 1.623(9) . ? 
Si19 O43 1.627(8) . ? 
Si20 O33 1.556(9) . ? 
Si20 O38 1.592(9) . ? 
Si20 O34 1.597(8) . ? 
Si20 O39 1.598(9) . ? 
Si21 O34 1.585(8) . ? 
Si21 O35 1.592(9) . ? 
Si21 O18 1.605(8) 4_566 ? 
Si21 O25 1.626(10) . ? 
Si22 O15 1.574(9) 4_566 ? 
Si22 O36 1.602(9) . ? 
Si22 O35 1.628(9) . ? 
Si22 O26 1.640(11) . ? 
Si23 O36 1.576(9) . ? 
Si23 O40 1.601(9) . ? 
Si23 O48 1.609(8) . ? 
Si23 O37 1.609(9) . ? 
Si24 O24 1.571(10) . ? 
Si24 O37 1.577(9) . ? 
Si24 O46 1.599(9) 4_666 ? 
Si24 O38 1.622(8) . ? 
O15 Si22 1.573(9) 4_665 ? 
O16 Si16 1.646(9) 4_665 ? 
O17 Si16 1.622(9) 4_665 ? 
O18 Si21 1.605(8) 4_665 ? 
O19 Si15 1.593(9) 4_665 ? 
O20 Si15 1.590(9) 4_665 ? 
O21 Si13 1.581(8) 2_545 ? 
O22 Si19 1.604(9) 2_545 ? 
O41 Si10 1.625(8) 4_666 ? 
O42 Si4 1.546(9) 4_666 ? 
O43 Si4 1.575(9) 4_666 ? 
O44 Si9 1.586(9) 4_666 ? 
O45 Si3 1.585(9) 4_666 ? 
O46 Si24 1.599(9) 4_565 ? 
O47 Si1 1.609(7) 2_545 ? 
O48 Si7 1.587(8) 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 123.8 . . ? 
C302 C303 C304 123.8 . . ? 
C102 C101 C103 104(5) 3_766 3_766 ? 
C102 C101 C102 25(4) 3_766 . ? 
C103 C101 C102 92(3) 3_766 . ? 
C102 C101 C104 153(4) 3_766 3_766 ? 
C103 C101 C104 57.3(16) 3_766 3_766 ? 
C102 C101 C104 149(2) . 3_766 ? 
C101 C102 C102 132(6) 3_766 3_766 ? 
C101 C102 C103 41(2) 3_766 . ? 
C102 C102 C103 106(3) 3_766 . ? 
C101 C102 C101 155(3) 3_766 . ? 
C102 C102 C101 23(4) 3_766 . ? 
C103 C102 C101 123.8 . . ? 
C101 C102 C103 153(3) 3_766 3_766 ? 
C102 C102 C103 46.3(16) 3_766 3_766 ? 
C103 C102 C103 153(2) . 3_766 ? 
C101 C102 C103 30.7(17) . 3_766 ? 
C101 C103 C102 35(3) 3_766 . ? 
C101 C103 C104 92(2) 3_766 . ? 
C102 C103 C104 123.8 . . ? 
C101 C103 C102 57.3(17) 3_766 3_766 ? 
C102 C103 C102 27.3(16) . 3_766 ? 
C104 C103 C102 149.3(13) . 3_766 ? 
C103 C104 C101 30.7(10) . 3_766 ? 
O16 Si1 O1 110.7(6) . . ? 
O16 Si1 O47 109.5(5) . 2 ? 
O1 Si1 O47 107.7(4) . 2 ? 
O16 Si1 O15 108.6(5) . . ? 
O1 Si1 O15 110.8(6) . . ? 
O47 Si1 O15 109.6(5) 2 . ? 
O6 Si2 O1 112.4(5) . . ? 
O6 Si2 O13 105.5(6) . . ? 
O1 Si2 O13 109.1(6) . . ? 
O6 Si2 O2 110.6(5) . . ? 
O1 Si2 O2 107.0(5) . . ? 
O13 Si2 O2 112.3(5) . . ? 
O45 Si3 O3 108.9(6) 4_565 . ? 
O45 Si3 O2 110.5(5) 4_565 . ? 
O3 Si3 O2 111.4(5) . . ? 
O45 Si3 O46 109.5(5) 4_565 . ? 
O3 Si3 O46 109.0(6) . . ? 
O2 Si3 O46 107.5(5) . . ? 
O42 Si4 O43 110.2(5) 4_565 4_565 ? 
O42 Si4 O3 109.7(6) 4_565 . ? 
O43 Si4 O3 109.1(6) 4_565 . ? 
O42 Si4 O4 109.2(5) 4_565 . ? 
O43 Si4 O4 108.3(5) 4_565 . ? 
O3 Si4 O4 110.3(5) . . ? 
O4 Si5 O14 108.2(5) . . ? 
O4 Si5 O5 110.6(5) . . ? 
O14 Si5 O5 111.3(5) . . ? 
O4 Si5 O21 109.4(5) . . ? 
O14 Si5 O21 111.7(5) . . ? 
O5 Si5 O21 105.7(5) . . ? 
O18 Si6 O19 109.2(5) . . ? 
O18 Si6 O6 110.5(5) . . ? 
O19 Si6 O6 110.4(6) . . ? 
O18 Si6 O5 107.8(5) . . ? 
O19 Si6 O5 109.3(5) . . ? 
O6 Si6 O5 109.5(4) . . ? 
O7 Si7 O17 108.8(5) . . ? 
O7 Si7 O48 107.6(5) . 2 ? 
O17 Si7 O48 113.0(5) . 2 ? 
O7 Si7 O23 109.2(5) . . ? 
O17 Si7 O23 107.2(4) . . ? 
O48 Si7 O23 111.0(4) 2 . ? 
O13 Si8 O12 107.6(6) . . ? 
O13 Si8 O8 112.3(5) . . ? 
O12 Si8 O8 111.5(5) . . ? 
O13 Si8 O7 109.7(6) . . ? 
O12 Si8 O7 108.3(5) . . ? 
O8 Si8 O7 107.4(5) . . ? 
O25 Si9 O8 107.2(4) . . ? 
O25 Si9 O44 108.4(4) . 4_565 ? 
O8 Si9 O44 110.3(5) . 4_565 ? 
O25 Si9 O9 110.6(4) . . ? 
O8 Si9 O9 109.4(5) . . ? 
O44 Si9 O9 110.9(5) 4_565 . ? 
O26 Si10 O9 110.9(4) . . ? 
O26 Si10 O10 109.1(4) . . ? 
O9 Si10 O10 109.7(5) . . ? 
O26 Si10 O41 107.9(4) . 4_565 ? 
O9 Si10 O41 108.8(5) . 4_565 ? 
O10 Si10 O41 110.5(6) . 4_565 ? 
O14 Si11 O22 111.3(5) . . ? 
O14 Si11 O11 109.5(5) . . ? 
O22 Si11 O11 108.5(5) . . ? 
O14 Si11 O10 107.7(5) . . ? 
O22 Si11 O10 107.7(5) . . ? 
O11 Si11 O10 112.2(5) . . ? 
O12 Si12 O11 110.3(5) . . ? 
O12 Si12 O20 107.4(5) . . ? 
O11 Si12 O20 109.3(5) . . ? 
O12 Si12 O24 111.0(4) . . ? 
O11 Si12 O24 110.9(4) . . ? 
O20 Si12 O24 107.9(4) . . ? 
O41 Si13 O21 107.2(5) . 2 ? 
O41 Si13 O27 108.4(6) . . ? 
O21 Si13 O27 109.2(5) 2 . ? 
O41 Si13 O42 111.1(5) . . ? 
O21 Si13 O42 109.9(5) 2 . ? 
O27 Si13 O42 111.0(5) . . ? 
O39 Si14 O27 110.9(6) . . ? 
O39 Si14 O28 109.1(5) . . ? 
O27 Si14 O28 108.6(5) . . ? 
O39 Si14 O32 111.6(6) . . ? 
O27 Si14 O32 108.3(5) . . ? 
O28 Si14 O32 108.2(5) . . ? 
O29 Si15 O20 110.4(6) . 4_566 ? 
O29 Si15 O28 109.9(5) . . ? 
O20 Si15 O28 108.7(5) 4_566 . ? 
O29 Si15 O19 109.1(6) . 4_566 ? 
O20 Si15 O19 110.8(5) 4_566 4_566 ? 
O28 Si15 O19 107.8(5) . 4_566 ? 
O30 Si16 O29 110.5(5) . . ? 
O30 Si16 O17 108.0(6) . 4_566 ? 
O29 Si16 O17 109.8(6) . 4_566 ? 
O30 Si16 O16 110.6(6) . 4_566 ? 
O29 Si16 O16 107.8(6) . 4_566 ? 
O17 Si16 O16 110.0(5) 4_566 4_566 ? 
O47 Si17 O31 109.4(5) . . ? 
O47 Si17 O40 110.3(5) . . ? 
O31 Si17 O40 109.0(5) . . ? 
O47 Si17 O30 110.0(5) . . ? 
O31 Si17 O30 108.6(5) . . ? 
O40 Si17 O30 109.4(5) . . ? 
O31 Si18 O32 109.7(4) . . ? 
O31 Si18 O45 108.8(6) . . ? 
O32 Si18 O45 110.3(5) . . ? 
O31 Si18 O44 108.5(5) . . ? 
O32 Si18 O44 110.1(5) . . ? 
O45 Si18 O44 109.4(5) . . ? 
O23 Si19 O22 110.4(4) . 2 ? 
O23 Si19 O33 109.6(5) . . ? 
O22 Si19 O33 108.4(5) 2 . ? 
O23 Si19 O43 108.3(4) . . ? 
O22 Si19 O43 108.4(5) 2 . ? 
O33 Si19 O43 111.8(5) . . ? 
O33 Si20 O38 111.9(5) . . ? 
O33 Si20 O34 108.4(5) . . ? 
O38 Si20 O34 107.4(5) . . ? 
O33 Si20 O39 110.4(6) . . ? 
O38 Si20 O39 110.8(6) . . ? 
O34 Si20 O39 107.9(5) . . ? 
O34 Si21 O35 108.5(5) . . ? 
O34 Si21 O18 109.2(4) . 4_566 ? 
O35 Si21 O18 107.0(5) . 4_566 ? 
O34 Si21 O25 112.2(4) . . ? 
O35 Si21 O25 110.8(4) . . ? 
O18 Si21 O25 109.0(4) 4_566 . ? 
O15 Si22 O36 110.8(6) 4_566 . ? 
O15 Si22 O35 109.9(5) 4_566 . ? 
O36 Si22 O35 108.6(6) . . ? 
O15 Si22 O26 108.1(4) 4_566 . ? 
O36 Si22 O26 109.2(5) . . ? 
O35 Si22 O26 110.3(4) . . ? 
O36 Si23 O40 109.9(5) . . ? 
O36 Si23 O48 110.4(5) . . ? 
O40 Si23 O48 109.4(5) . . ? 
O36 Si23 O37 108.0(6) . . ? 
O40 Si23 O37 110.2(5) . . ? 
O48 Si23 O37 108.9(5) . . ? 
O24 Si24 O37 108.6(4) . . ? 
O24 Si24 O46 107.3(4) . 4_666 ? 
O37 Si24 O46 112.6(5) . 4_666 ? 
O24 Si24 O38 108.5(4) . . ? 
O37 Si24 O38 106.7(5) . . ? 
O46 Si24 O38 113.0(5) 4_666 . ? 
Si2 O1 Si1 150.3(7) . . ? 
Si3 O2 Si2 148.8(6) . . ? 
Si3 O3 Si4 171.8(8) . . ? 
Si5 O4 Si4 154.0(7) . . ? 
Si6 O5 Si5 145.3(6) . . ? 
Si2 O6 Si6 164.4(7) . . ? 
Si7 O7 Si8 158.7(7) . . ? 
Si9 O8 Si8 154.4(6) . . ? 
Si10 O9 Si9 152.1(5) . . ? 
Si10 O10 Si11 159.1(7) . . ? 
Si12 O11 Si11 152.4(6) . . ? 
Si12 O12 Si8 173.9(7) . . ? 
Si8 O13 Si2 174.4(8) . . ? 
Si11 O14 Si5 162.3(6) . . ? 
Si22 O15 Si1 147.7(6) 4_665 . ? 
Si1 O16 Si16 172.0(8) . 4_665 ? 
Si7 O17 Si16 147.2(6) . 4_665 ? 
Si6 O18 Si21 145.5(6) . 4_665 ? 
Si6 O19 Si15 161.9(7) . 4_665 ? 
Si15 O20 Si12 145.8(6) 4_665 . ? 
Si13 O21 Si5 146.4(6) 2_545 . ? 
Si11 O22 Si19 151.8(6) . 2_545 ? 
Si19 O23 Si7 155.5(3) . . ? 
Si24 O24 Si12 150.2(3) . . ? 
Si9 O25 Si21 153.4(3) . . ? 
Si10 O26 Si22 145.7(3) . . ? 
Si14 O27 Si13 153.1(7) . . ? 
Si15 O28 Si14 152.4(6) . . ? 
Si15 O29 Si16 174.3(8) . . ? 
Si16 O30 Si17 157.6(8) . . ? 
Si17 O31 Si18 150.3(6) . . ? 
Si14 O32 Si18 156.6(6) . . ? 
Si20 O33 Si19 153.6(7) . . ? 
Si21 O34 Si20 153.3(6) . . ? 
Si21 O35 Si22 151.8(6) . . ? 
Si23 O36 Si22 163.4(7) . . ? 
Si24 O37 Si23 153.1(6) . . ? 
Si20 O38 Si24 157.1(7) . . ? 
Si14 O39 Si20 176.2(7) . . ? 
Si17 O40 Si23 165.9(6) . . ? 
Si13 O41 Si10 148.1(6) . 4_666 ? 
Si4 O42 Si13 163.3(7) 4_666 . ? 
Si4 O43 Si19 148.6(6) 4_666 . ? 
Si9 O44 Si18 147.0(6) 4_666 . ? 
Si3 O45 Si18 161.4(8) 4_666 . ? 
Si24 O46 Si3 150.1(6) 4_565 . ? 
Si17 O47 Si1 148.9(5) . 2_545 ? 
Si7 O48 Si23 147.6(6) 2_545 . ? 
  
_diffrn_measured_fraction_theta_max    0.939 
_diffrn_reflns_theta_full              28.60 
_diffrn_measured_fraction_theta_full   0.939 
_refine_diff_density_max    0.920 
_refine_diff_density_min   -0.473 
_refine_diff_density_rms    0.139 


