# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_finalorth2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H51 O P Si4 W'
_chemical_formula_weight         622.78

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'
P P 0.1023 0.0942 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'p n a 21'

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

_cell_length_a                   17.903(4)
_cell_length_b                   10.516(2)
_cell_length_c                   17.191(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3236.6(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    3.773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3973
_exptl_absorpt_correction_T_max  0.5191
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32436
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         28.34
_reflns_number_total             7734
_reflns_number_gt                5615
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F^2^, conventional R-factors R are based
 on F, with F set to zero for negative F^2^. The threshold expression of
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.025(10)
_refine_ls_number_reflns         7734
_refine_ls_number_parameters     251
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0782
_refine_ls_wR_factor_gt          0.0695
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_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
C1 C 0.6792(6) 0.5739(8) 0.8320(5) 0.050(2) Uani 1 1 d . . .
H1A H 0.6930 0.6248 0.8769 0.060 Uiso 1 1 calc R . .
H1B H 0.6343 0.6112 0.8101 0.060 Uiso 1 1 calc R . .
C2 C 0.7870(4) 0.7662(6) 0.6968(4) 0.0479(15) Uani 1 1 d . . .
H2A H 0.8407 0.7728 0.6901 0.057 Uiso 1 1 calc R . .
H2B H 0.7653 0.7640 0.6450 0.057 Uiso 1 1 calc R . .
C3 C 0.7987(4) 0.4243(6) 0.6888(4) 0.0559(17) Uani 1 1 d . . .
H3A H 0.8161 0.3638 0.7273 0.067 Uiso 1 1 calc R . .
H3B H 0.7544 0.3880 0.6651 0.067 Uiso 1 1 calc R . .
O1 O 0.6658(5) 0.5841(7) 0.6635(4) 0.071(2) Uani 1 1 d . . .
C5 C 0.6139(5) 0.3124(8) 0.7884(5) 0.088(3) Uani 1 1 d . . .
H5A H 0.6479 0.3076 0.7453 0.132 Uiso 1 1 calc R . .
H5B H 0.5680 0.3508 0.7715 0.132 Uiso 1 1 calc R . .
H5C H 0.6040 0.2284 0.8076 0.132 Uiso 1 1 calc R . .
C6 C 0.7380(5) 0.3209(10) 0.9042(7) 0.101(4) Uani 1 1 d . . .
H6A H 0.7217 0.2417 0.9262 0.152 Uiso 1 1 calc R . .
H6B H 0.7626 0.3705 0.9435 0.152 Uiso 1 1 calc R . .
H6C H 0.7720 0.3046 0.8622 0.152 Uiso 1 1 calc R . .
C7 C 0.5845(9) 0.4197(11) 0.9481(7) 0.106(5) Uani 1 1 d . . .
H7A H 0.5750 0.3360 0.9682 0.159 Uiso 1 1 calc R . .
H7B H 0.5389 0.4552 0.9284 0.159 Uiso 1 1 calc R . .
H7C H 0.6035 0.4728 0.9890 0.159 Uiso 1 1 calc R . .
C8 C 0.8057(12) 0.9384(17) 0.8347(11) 0.270(14) Uani 1 1 d . . .
H8A H 0.7710 0.9405 0.8773 0.404 Uiso 1 1 calc R . .
H8B H 0.8327 1.0173 0.8327 0.404 Uiso 1 1 calc R . .
H8C H 0.8402 0.8695 0.8420 0.404 Uiso 1 1 calc R . .
C9 C 0.7762(8) 1.0521(10) 0.6800(10) 0.173(7) Uani 1 1 d . . .
H9A H 0.8237 1.0877 0.6943 0.260 Uiso 1 1 calc R . .
H9B H 0.7381 1.1156 0.6855 0.260 Uiso 1 1 calc R . .
H9C H 0.7781 1.0239 0.6269 0.260 Uiso 1 1 calc R . .
C10 C 0.6532(5) 0.9114(8) 0.7586(15) 0.207(10) Uani 1 1 d . . .
H10A H 0.6385 0.9807 0.7915 0.311 Uiso 1 1 calc R . .
H10B H 0.6395 0.8324 0.7826 0.311 Uiso 1 1 calc R . .
H10C H 0.6286 0.9189 0.7092 0.311 Uiso 1 1 calc R . .
C11 C 0.8369(9) 0.5342(15) 0.5305(6) 0.174(7) Uani 1 1 d . . .
H11A H 0.8761 0.5898 0.5133 0.261 Uiso 1 1 calc R . .
H11B H 0.7950 0.5838 0.5475 0.261 Uiso 1 1 calc R . .
H11C H 0.8219 0.4802 0.4883 0.261 Uiso 1 1 calc R . .
C12 C 0.8958(9) 0.2807(10) 0.5755(8) 0.208(9) Uani 1 1 d . . .
H12A H 0.8525 0.2415 0.5530 0.312 Uiso 1 1 calc R . .
H12B H 0.9142 0.2288 0.6173 0.312 Uiso 1 1 calc R . .
H12C H 0.9339 0.2895 0.5365 0.312 Uiso 1 1 calc R . .
C13 C 0.9591(6) 0.5070(17) 0.6514(8) 0.172(7) Uani 1 1 d . . .
H13A H 0.9468 0.5745 0.6867 0.258 Uiso 1 1 calc R . .
H13B H 0.9882 0.5403 0.6092 0.258 Uiso 1 1 calc R . .
H13C H 0.9874 0.4431 0.6783 0.258 Uiso 1 1 calc R . .
C17 C 0.5953(9) 0.4354(11) 0.5587(7) 0.104(5) Uani 1 1 d . . .
H17A H 0.6438 0.4134 0.5389 0.156 Uiso 1 1 calc R . .
H17B H 0.5609 0.4439 0.5162 0.156 Uiso 1 1 calc R . .
H17C H 0.5783 0.3699 0.5933 0.156 Uiso 1 1 calc R . .
C18 C 0.6042(5) 0.7054(10) 0.5408(6) 0.122(4) Uani 1 1 d . . .
H18A H 0.6100 0.7857 0.5667 0.182 Uiso 1 1 calc R . .
H18B H 0.5587 0.7057 0.5113 0.182 Uiso 1 1 calc R . .
H18C H 0.6457 0.6917 0.5065 0.182 Uiso 1 1 calc R . .
C19 C 0.5140(5) 0.5993(9) 0.6564(6) 0.090(3) Uani 1 1 d . . .
H19A H 0.5066 0.5298 0.6918 0.135 Uiso 1 1 calc R . .
H19B H 0.4750 0.5991 0.6180 0.135 Uiso 1 1 calc R . .
H19C H 0.5127 0.6780 0.6847 0.135 Uiso 1 1 calc R . .
C14 C 0.9811(4) 0.7243(9) 0.8706(6) 0.095(3) Uani 1 1 d . . .
H14A H 0.9963 0.7234 0.8170 0.143 Uiso 1 1 calc R . .
H14B H 1.0242 0.7145 0.9033 0.143 Uiso 1 1 calc R . .
H14C H 0.9570 0.8036 0.8821 0.143 Uiso 1 1 calc R . .
C15 C 0.9674(6) 0.4365(10) 0.8854(6) 0.109(4) Uani 1 1 d . . .
H15A H 0.9946 0.4307 0.8374 0.163 Uiso 1 1 calc R . .
H15B H 0.9326 0.3673 0.8887 0.163 Uiso 1 1 calc R . .
H15C H 1.0015 0.4324 0.9283 0.163 Uiso 1 1 calc R . .
C16 C 0.8733(7) 0.6054(11) 0.9884(5) 0.109(4) Uani 1 1 d . . .
H16A H 0.9113 0.6305 1.0248 0.164 Uiso 1 1 calc R . .
H16B H 0.8530 0.5248 1.0038 0.164 Uiso 1 1 calc R . .
H16C H 0.8343 0.6681 0.9878 0.164 Uiso 1 1 calc R . .
C4 C 0.8409(4) 0.5928(6) 0.8144(4) 0.0509(16) Uani 1 1 d . . .
Si4 Si 0.91517(12) 0.5915(2) 0.88864(13) 0.0649(6) Uani 1 1 d . . .
Si1 Si 0.65574(12) 0.40984(19) 0.86683(12) 0.0581(5) Uani 1 1 d . . .
Si2 Si 0.75490(11) 0.91581(15) 0.7440(4) 0.0660(7) Uani 1 1 d . . .
Si3 Si 0.87131(13) 0.43490(19) 0.61237(13) 0.0641(6) Uani 1 1 d . . .
P1 P 0.60103(11) 0.58294(19) 0.61030(11) 0.0585(5) Uani 1 1 d . . .
W1 W 0.765341(10) 0.589555(16) 0.74878(3) 0.03504(6) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.059(6) 0.047(5) 0.044(4) -0.009(4) 0.017(4) -0.003(4)
C2 0.050(4) 0.045(4) 0.049(4) 0.002(3) 0.003(3) -0.006(3)
C3 0.062(4) 0.046(4) 0.060(4) 0.001(3) 0.023(4) 0.003(3)
O1 0.064(5) 0.086(5) 0.064(4) 0.005(4) -0.022(3) -0.010(3)
C5 0.106(7) 0.073(6) 0.085(6) 0.015(4) 0.009(5) -0.032(5)
C6 0.086(6) 0.097(7) 0.121(9) 0.069(7) 0.021(6) 0.021(5)
C7 0.113(11) 0.109(9) 0.094(8) 0.001(7) 0.055(8) -0.001(8)
C8 0.32(3) 0.213(18) 0.27(2) -0.205(18) -0.15(2) 0.157(18)
C9 0.236(17) 0.039(5) 0.245(18) 0.036(8) 0.097(14) 0.009(7)
C10 0.074(7) 0.070(6) 0.48(3) -0.046(15) 0.100(18) 0.007(4)
C11 0.200(16) 0.253(17) 0.070(7) 0.063(9) 0.075(9) 0.084(13)
C12 0.29(2) 0.102(9) 0.228(16) -0.048(9) 0.216(15) -0.013(10)
C13 0.074(8) 0.32(2) 0.126(11) -0.036(14) 0.045(8) -0.056(11)
C17 0.117(12) 0.108(9) 0.088(8) -0.032(7) -0.034(8) -0.008(8)
C18 0.086(7) 0.168(11) 0.110(8) 0.078(8) -0.030(6) -0.038(7)
C19 0.073(6) 0.129(9) 0.067(6) -0.008(6) -0.004(4) 0.013(5)
C14 0.068(6) 0.131(9) 0.087(7) 0.016(6) -0.020(5) -0.035(6)
C15 0.076(7) 0.166(11) 0.084(7) 0.044(7) 0.006(6) 0.048(7)
C16 0.117(9) 0.169(11) 0.042(5) 0.018(6) -0.021(5) -0.030(7)
C4 0.042(4) 0.071(4) 0.039(3) 0.009(4) 0.004(3) -0.003(3)
Si4 0.0509(12) 0.0970(16) 0.0468(11) 0.0136(13) -0.0105(9) -0.0089(11)
Si1 0.0544(12) 0.0617(12) 0.0583(12) 0.0139(11) 0.0192(9) -0.0015(10)
Si2 0.0708(11) 0.0412(8) 0.0859(19) 0.007(3) 0.021(2) 0.0018(7)
Si3 0.0705(14) 0.0637(14) 0.0582(13) -0.0058(11) 0.0310(11) 0.0002(10)
P1 0.0499(11) 0.0823(13) 0.0433(10) 0.0006(11) -0.0090(8) -0.0105(9)
W1 0.03366(10) 0.03818(10) 0.03329(10) 0.0000(5) 0.0026(2) -0.00093(8)

_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
C1 Si1 1.874(9) . ?
C1 W1 2.110(10) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 Si2 1.862(7) . ?
C2 W1 2.097(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 Si3 1.852(7) . ?
C3 W1 2.107(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
O1 P1 1.478(7) . ?
O1 W1 2.307(7) . ?
C5 Si1 1.852(8) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 Si1 1.858(8) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 Si1 1.895(13) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 Si2 1.821(16) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 Si2 1.847(12) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 Si2 1.838(9) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 Si3 1.857(12) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 Si3 1.795(10) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 Si3 1.870(12) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C17 P1 1.790(10) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 P1 1.757(9) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 P1 1.757(9) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C14 Si4 1.854(8) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 Si4 1.880(10) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 Si4 1.878(10) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C4 W1 1.763(7) . ?
C4 Si4 1.842(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Si1 C1 W1 116.9(4) . . ?
Si1 C1 H1A 108.1 . . ?
W1 C1 H1A 108.1 . . ?
Si1 C1 H1B 108.1 . . ?
W1 C1 H1B 108.1 . . ?
H1A C1 H1B 107.3 . . ?
Si2 C2 W1 120.3(3) . . ?
Si2 C2 H2A 107.2 . . ?
W1 C2 H2A 107.2 . . ?
Si2 C2 H2B 107.2 . . ?
W1 C2 H2B 107.2 . . ?
H2A C2 H2B 106.9 . . ?
Si3 C3 W1 119.8(3) . . ?
Si3 C3 H3A 107.4 . . ?
W1 C3 H3A 107.4 . . ?
Si3 C3 H3B 107.4 . . ?
W1 C3 H3B 107.4 . . ?
H3A C3 H3B 106.9 . . ?
P1 O1 W1 178.5(5) . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si3 C13 H13A 109.5 . . ?
Si3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
P1 C17 H17A 109.5 . . ?
P1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
P1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
P1 C18 H18A 109.5 . . ?
P1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
P1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
P1 C19 H19A 109.5 . . ?
P1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
P1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si4 C14 H14A 109.5 . . ?
Si4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si4 C15 H15A 109.5 . . ?
Si4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si4 C16 H16A 109.5 . . ?
Si4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
W1 C4 Si4 175.7(4) . . ?
C4 Si4 C14 109.7(4) . . ?
C4 Si4 C16 110.1(4) . . ?
C14 Si4 C16 110.4(5) . . ?
C4 Si4 C15 110.2(4) . . ?
C14 Si4 C15 109.4(5) . . ?
C16 Si4 C15 107.0(5) . . ?
C5 Si1 C6 107.1(5) . . ?
C5 Si1 C1 111.6(4) . . ?
C6 Si1 C1 113.4(5) . . ?
C5 Si1 C7 107.2(5) . . ?
C6 Si1 C7 107.8(5) . . ?
C1 Si1 C7 109.6(5) . . ?
C8 Si2 C10 112.4(10) . . ?
C8 Si2 C9 107.8(8) . . ?
C10 Si2 C9 107.8(7) . . ?
C8 Si2 C2 109.3(5) . . ?
C10 Si2 C2 110.1(5) . . ?
C9 Si2 C2 109.4(6) . . ?
C12 Si3 C3 111.6(4) . . ?
C12 Si3 C11 108.7(7) . . ?
C3 Si3 C11 109.8(5) . . ?
C12 Si3 C13 106.7(8) . . ?
C3 Si3 C13 111.1(4) . . ?
C11 Si3 C13 108.8(8) . . ?
O1 P1 C19 114.6(4) . . ?
O1 P1 C18 112.9(4) . . ?
C19 P1 C18 105.3(5) . . ?
O1 P1 C17 111.0(6) . . ?
C19 P1 C17 105.0(6) . . ?
C18 P1 C17 107.5(6) . . ?
C4 W1 C2 96.5(3) . . ?
C4 W1 C3 96.4(3) . . ?
C2 W1 C3 118.0(3) . . ?
C4 W1 C1 97.4(4) . . ?
C2 W1 C1 119.5(3) . . ?
C3 W1 C1 118.4(3) . . ?
C4 W1 O1 179.5(3) . . ?
C2 W1 O1 83.9(3) . . ?
C3 W1 O1 83.6(3) . . ?
C1 W1 O1 82.2(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W1 C4 Si4 C14 -148(6) . . . . ?
W1 C4 Si4 C16 -26(6) . . . . ?
W1 C4 Si4 C15 92(6) . . . . ?
W1 C1 Si1 C5 -67.2(7) . . . . ?
W1 C1 Si1 C6 53.7(7) . . . . ?
W1 C1 Si1 C7 174.2(6) . . . . ?
W1 C2 Si2 C8 66.6(10) . . . . ?
W1 C2 Si2 C10 -57.4(10) . . . . ?
W1 C2 Si2 C9 -175.6(6) . . . . ?
W1 C3 Si3 C12 175.2(7) . . . . ?
W1 C3 Si3 C11 -64.2(8) . . . . ?
W1 C3 Si3 C13 56.2(8) . . . . ?
W1 O1 P1 C19 -32(20) . . . . ?
W1 O1 P1 C18 88(20) . . . . ?
W1 O1 P1 C17 -151(19) . . . . ?
Si4 C4 W1 C2 138(6) . . . . ?
Si4 C4 W1 C3 -103(6) . . . . ?
Si4 C4 W1 C1 17(6) . . . . ?
Si4 C4 W1 O1 -16(43) . . . . ?
Si2 C2 W1 C4 -82.2(4) . . . . ?
Si2 C2 W1 C3 177.0(4) . . . . ?
Si2 C2 W1 C1 20.1(6) . . . . ?
Si2 C2 W1 O1 97.6(4) . . . . ?
Si3 C3 W1 C4 -80.6(5) . . . . ?
Si3 C3 W1 C2 20.3(6) . . . . ?
Si3 C3 W1 C1 177.4(5) . . . . ?
Si3 C3 W1 O1 99.9(5) . . . . ?
Si1 C1 W1 C4 -85.3(6) . . . . ?
Si1 C1 W1 C2 172.8(4) . . . . ?
Si1 C1 W1 C3 16.1(7) . . . . ?
Si1 C1 W1 O1 94.4(6) . . . . ?
P1 O1 W1 C4 76(42) . . . . ?
P1 O1 W1 C2 -78(20) . . . . ?
P1 O1 W1 C3 163(20) . . . . ?
P1 O1 W1 C1 43(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.821
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.116
_database_code_depnum_ccdc_archive 'CCDC 949733'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_t1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H90 O9 Si6 W3'
_chemical_formula_weight         1387.17

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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I -4 3 d'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+3/4'
'z+1/4, y+1/4, x+1/4'
'z+3/4, -y+1/4, -x+3/4'
'-z+3/4, y+3/4, -x+1/4'
'-z+1/4, -y+3/4, x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+5/4'
'z+3/4, y+3/4, x+3/4'
'z+5/4, -y+3/4, -x+5/4'
'-z+5/4, y+5/4, -x+3/4'
'-z+3/4, -y+5/4, x+5/4'

_cell_length_a                   28.065(3)
_cell_length_b                   28.065(3)
_cell_length_c                   28.065(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     22105(4)
_cell_formula_units_Z            16
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10944
_exptl_absorpt_coefficient_mu    6.400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4469
_exptl_absorpt_correction_T_max  0.6629
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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-AXS Smart APEX II'
_diffrn_measurement_method       '\w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            67995
_diffrn_reflns_av_R_equivalents  0.1358
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         28.61
_reflns_number_total             4603
_reflns_number_gt                4285
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.020(7)
_refine_ls_number_reflns         4603
_refine_ls_number_parameters     169
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0218
_refine_ls_wR_factor_ref         0.0490
_refine_ls_wR_factor_gt          0.0480
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.009
_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
W1 W 1.012543(5) 0.442460(5) 0.946156(5) 0.01326(4) Uani 1 1 d . . .
O1 O 0.96278(10) 0.43185(9) 0.87907(10) 0.0209(6) Uani 1 1 d . . .
C1 C 0.95341(17) 0.38657(15) 0.85723(16) 0.0299(10) Uani 1 1 d . . .
H1A H 0.9318 0.3679 0.8767 0.036 Uiso 1 1 calc R . .
H1B H 0.9828 0.3688 0.8531 0.036 Uiso 1 1 calc R . .
C2 C 0.93090(16) 0.39773(15) 0.80897(16) 0.0307(10) Uani 1 1 d . . .
H2A H 0.9054 0.3756 0.8017 0.037 Uiso 1 1 calc R . .
H2B H 0.9544 0.3965 0.7837 0.037 Uiso 1 1 calc R . .
C4 C 0.92172(16) 0.46082(16) 0.86645(15) 0.0286(9) Uani 1 1 d . . .
H4A H 0.9289 0.4945 0.8699 0.034 Uiso 1 1 calc R . .
H4B H 0.8946 0.4531 0.8865 0.034 Uiso 1 1 calc R . .
C3 C 0.91154(18) 0.44872(16) 0.81535(16) 0.0344(11) Uani 1 1 d . . .
H3A H 0.9276 0.4707 0.7941 0.041 Uiso 1 1 calc R . .
H3B H 0.8776 0.4498 0.8090 0.041 Uiso 1 1 calc R . .
Si2 Si 0.96166(4) 0.34182(4) 0.99585(4) 0.0198(2) Uani 1 1 d . . .
Si1 Si 1.08693(4) 0.47889(4) 0.85476(4) 0.0198(2) Uani 1 1 d . . .
C7 C 0.91161(15) 0.32611(18) 1.03775(17) 0.0357(11) Uani 1 1 d . . .
H7A H 0.9125 0.3469 1.0649 0.054 Uiso 1 1 calc R . .
H7B H 0.9151 0.2937 1.0481 0.054 Uiso 1 1 calc R . .
H7C H 0.8817 0.3297 1.0216 0.054 Uiso 1 1 calc R . .
C5 C 1.01907(15) 0.33181(15) 1.02825(16) 0.0287(10) Uani 1 1 d . . .
H5A H 1.0452 0.3403 1.0079 0.043 Uiso 1 1 calc R . .
H5B H 1.0216 0.2988 1.0370 0.043 Uiso 1 1 calc R . .
H5C H 1.0198 0.3512 1.0564 0.043 Uiso 1 1 calc R . .
C6 C 0.95972(15) 0.29992(14) 0.94418(17) 0.0297(10) Uani 1 1 d . . .
H6A H 0.9311 0.3053 0.9262 0.045 Uiso 1 1 calc R . .
H6B H 0.9602 0.2677 0.9556 0.045 Uiso 1 1 calc R . .
H6C H 0.9869 0.3053 0.9241 0.045 Uiso 1 1 calc R . .
C10 C 1.09630(16) 0.52992(15) 0.81355(15) 0.0277(9) Uani 1 1 d . . .
H10A H 1.0684 0.5342 0.7942 0.042 Uiso 1 1 calc R . .
H10B H 1.1233 0.5236 0.7935 0.042 Uiso 1 1 calc R . .
H10C H 1.1020 0.5583 0.8317 0.042 Uiso 1 1 calc R . .
C9 C 1.14220(15) 0.46651(17) 0.88982(16) 0.0306(10) Uani 1 1 d . . .
H9A H 1.1673 0.4569 0.8686 0.046 Uiso 1 1 calc R . .
H9B H 1.1361 0.4415 0.9123 0.046 Uiso 1 1 calc R . .
H9C H 1.1517 0.4948 0.9066 0.046 Uiso 1 1 calc R . .
C8 C 1.07340(19) 0.42557(16) 0.81754(18) 0.0400(13) Uani 1 1 d . . .
H8A H 1.0442 0.4307 0.8006 0.060 Uiso 1 1 calc R . .
H8B H 1.0703 0.3981 0.8377 0.060 Uiso 1 1 calc R . .
H8C H 1.0988 0.4205 0.7952 0.060 Uiso 1 1 calc R . .
C11 C 0.95264(14) 0.40528(13) 0.97767(14) 0.0182(8) Uani 1 1 d . . .
H11A H 0.9427 0.4230 1.0056 0.022 Uiso 1 1 calc R . .
H11B H 0.9265 0.4062 0.9551 0.022 Uiso 1 1 calc R . .
C12 C 1.03616(14) 0.49468(13) 0.89483(13) 0.0178(8) Uani 1 1 d . . .
H12A H 1.0091 0.5028 0.8749 0.021 Uiso 1 1 calc R . .
H12B H 1.0449 0.5233 0.9122 0.021 Uiso 1 1 calc R . .
O4 O 1.04301(9) 0.46092(9) 0.99770(9) 0.0161(6) Uani 1 1 d . . .
O5 O 1.04346(9) 0.39395(9) 0.92593(9) 0.0179(5) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.01412(7) 0.01276(7) 0.01291(7) -0.00009(6) 0.00043(6) -0.00021(6)
O1 0.0228(14) 0.0198(14) 0.0202(13) -0.0041(11) -0.0027(12) 0.0038(11)
C1 0.036(3) 0.022(2) 0.031(2) -0.0041(18) -0.007(2) -0.0021(19)
C2 0.034(2) 0.031(2) 0.028(2) -0.0113(19) -0.0066(19) -0.0044(19)
C4 0.030(2) 0.029(2) 0.026(2) -0.0037(19) -0.0084(19) 0.0072(19)
C3 0.043(3) 0.031(2) 0.029(2) -0.006(2) -0.012(2) 0.004(2)
Si2 0.0175(5) 0.0168(5) 0.0252(6) 0.0053(4) -0.0018(4) -0.0018(4)
Si1 0.0238(5) 0.0184(5) 0.0171(5) 0.0001(4) 0.0050(4) -0.0019(5)
C7 0.023(2) 0.048(3) 0.036(2) 0.018(2) 0.000(2) -0.007(2)
C5 0.026(2) 0.021(2) 0.039(2) 0.0053(18) -0.0110(19) 0.0002(18)
C6 0.026(2) 0.020(2) 0.043(3) -0.005(2) -0.010(2) 0.0023(17)
C10 0.031(2) 0.028(2) 0.024(2) 0.0051(18) 0.0034(18) -0.0053(19)
C9 0.021(2) 0.039(3) 0.032(2) 0.006(2) 0.0095(18) 0.0042(19)
C8 0.059(3) 0.029(2) 0.031(3) -0.010(2) 0.020(2) -0.006(2)
C11 0.0199(19) 0.0168(18) 0.0178(18) 0.0027(15) -0.0006(15) -0.0016(15)
C12 0.0221(18) 0.0166(18) 0.0147(17) -0.0025(14) -0.0017(15) -0.0004(16)
O4 0.0165(13) 0.0186(12) 0.0134(12) 0.0013(11) 0.0023(10) 0.0002(11)
O5 0.0195(13) 0.0153(13) 0.0190(13) -0.0023(11) 0.0029(11) -0.0007(11)

_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
W1 O5 1.711(3) . ?
W1 O4 1.758(3) . ?
W1 C12 2.159(4) . ?
W1 C11 2.167(4) . ?
W1 O4 2.239(2) 11_567 ?
W1 O1 2.363(3) . ?
O1 C1 1.435(5) . ?
O1 C4 1.454(5) . ?
C1 C2 1.527(6) . ?
C2 C3 1.541(6) . ?
C4 C3 1.501(6) . ?
Si2 C6 1.868(4) . ?
Si2 C11 1.870(4) . ?
Si2 C5 1.871(4) . ?
Si2 C7 1.884(5) . ?
Si1 C10 1.859(4) . ?
Si1 C8 1.864(4) . ?
Si1 C12 1.869(4) . ?
Si1 C9 1.869(4) . ?
O4 W1 2.239(2) 8_746 ?

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
O5 W1 O4 105.11(13) . . ?
O5 W1 C12 99.39(13) . . ?
O4 W1 C12 101.52(13) . . ?
O5 W1 C11 98.38(13) . . ?
O4 W1 C11 100.56(13) . . ?
C12 W1 C11 146.83(14) . . ?
O5 W1 O4 165.93(11) . 11_567 ?
O4 W1 O4 88.97(15) . 11_567 ?
C12 W1 O4 77.30(11) . 11_567 ?
C11 W1 O4 78.68(12) . 11_567 ?
O5 W1 O1 86.28(11) . . ?
O4 W1 O1 168.51(11) . . ?
C12 W1 O1 74.65(12) . . ?
C11 W1 O1 78.81(12) . . ?
O4 W1 O1 79.65(9) 11_567 . ?
C1 O1 C4 104.2(3) . . ?
C1 O1 W1 124.1(2) . . ?
C4 O1 W1 126.3(2) . . ?
O1 C1 C2 105.8(3) . . ?
C1 C2 C3 103.5(3) . . ?
O1 C4 C3 104.9(3) . . ?
C4 C3 C2 104.7(3) . . ?
C6 Si2 C11 112.57(19) . . ?
C6 Si2 C5 107.93(19) . . ?
C11 Si2 C5 113.09(18) . . ?
C6 Si2 C7 108.4(2) . . ?
C11 Si2 C7 107.0(2) . . ?
C5 Si2 C7 107.7(2) . . ?
C10 Si1 C8 107.4(2) . . ?
C10 Si1 C12 107.43(18) . . ?
C8 Si1 C12 111.9(2) . . ?
C10 Si1 C9 110.7(2) . . ?
C8 Si1 C9 108.3(2) . . ?
C12 Si1 C9 111.10(18) . . ?
Si2 C11 W1 117.71(19) . . ?
Si1 C12 W1 118.33(19) . . ?
W1 O4 W1 150.90(15) . 8_746 ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        28.61
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.167
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.111
_database_code_depnum_ccdc_archive 'CCDC 949734'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_wa

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H84 O2 Si8 W2'
_chemical_formula_weight         1081.40

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'
W W -0.8490 6.8722 '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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   16.1077(7)
_cell_length_b                   16.1077(7)
_cell_length_c                   68.397(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     15368.5(13)
_cell_formula_units_Z            12
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       fragment
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6552
_exptl_absorpt_coefficient_mu    4.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3428
_exptl_absorpt_correction_T_max  0.5393
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            46502
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -91
_diffrn_reflns_limit_l_max       91
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         28.28
_reflns_number_total             8397
_reflns_number_gt                5689
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, Bruker (2000)'
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'

_refine_special_details          
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+126.6670P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8397
_refine_ls_number_parameters     275
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0306
_refine_ls_wR_factor_ref         0.0850
_refine_ls_wR_factor_gt          0.0664
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_restrained_S_all      0.877
_refine_ls_shift/su_max          0.080
_refine_ls_shift/su_mean         0.005

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
C1 C 0.6667 0.3333 0.15414(12) 0.0341(19) Uani 1 3 d S . .
C2 C 0.6390(5) 0.4261(5) 0.11809(8) 0.0610(18) Uani 1 1 d . . .
H2A H 0.5771 0.4121 0.1227 0.092 Uiso 1 1 calc R . .
H2B H 0.6389 0.4255 0.1041 0.092 Uiso 1 1 calc R . .
H2C H 0.6867 0.4882 0.1227 0.092 Uiso 1 1 calc R . .
C3 C 0.7708(4) 0.4767(3) 0.18595(7) 0.0340(11) Uani 1 1 d . . .
H3A H 0.7415 0.5149 0.1827 0.041 Uiso 1 1 calc R . .
H3B H 0.7810 0.4819 0.2000 0.041 Uiso 1 1 calc R . .
C4 C 0.8867(4) 0.5961(4) 0.15131(8) 0.0498(15) Uani 1 1 d . . .
H4A H 0.9480 0.6249 0.1449 0.075 Uiso 1 1 calc R . .
H4B H 0.8704 0.6445 0.1542 0.075 Uiso 1 1 calc R . .
H4C H 0.8389 0.5486 0.1429 0.075 Uiso 1 1 calc R . .
C5 C 0.9402(4) 0.4579(4) 0.16858(9) 0.0542(16) Uani 1 1 d . . .
H5A H 0.8984 0.4100 0.1594 0.081 Uiso 1 1 calc R . .
H5B H 0.9442 0.4273 0.1803 0.081 Uiso 1 1 calc R . .
H5C H 1.0030 0.4947 0.1629 0.081 Uiso 1 1 calc R . .
C6 C 0.9760(4) 0.6305(4) 0.19232(9) 0.0564(16) Uani 1 1 d . . .
H6A H 0.9772 0.5996 0.2042 0.085 Uiso 1 1 calc R . .
H6B H 0.9543 0.6751 0.1950 0.085 Uiso 1 1 calc R . .
H6C H 1.0393 0.6642 0.1868 0.085 Uiso 1 1 calc R . .
C7 C 0.7283(3) 0.2453(3) 0.24473(7) 0.0288(10) Uani 1 1 d . . .
H7A H 0.7056 0.2075 0.2566 0.035 Uiso 1 1 calc R . .
H7B H 0.7032 0.2010 0.2338 0.035 Uiso 1 1 calc R . .
C8 C 0.9144(4) 0.3836(4) 0.22273(8) 0.0491(14) Uani 1 1 d . . .
H8A H 0.9823 0.4082 0.2222 0.074 Uiso 1 1 calc R . .
H8B H 0.9022 0.4359 0.2239 0.074 Uiso 1 1 calc R . .
H8C H 0.8850 0.3482 0.2110 0.074 Uiso 1 1 calc R . .
C9 C 0.8911(5) 0.2042(5) 0.24255(11) 0.0638(19) Uani 1 1 d . . .
H9A H 0.8626 0.1676 0.2309 0.096 Uiso 1 1 calc R . .
H9B H 0.8655 0.1633 0.2538 0.096 Uiso 1 1 calc R . .
H9C H 0.9593 0.2305 0.2421 0.096 Uiso 1 1 calc R . .
C10 C 0.9182(4) 0.3733(5) 0.26705(8) 0.0503(15) Uani 1 1 d . . .
H10A H 0.9866 0.4018 0.2664 0.075 Uiso 1 1 calc R . .
H10B H 0.8941 0.3315 0.2782 0.075 Uiso 1 1 calc R . .
H10C H 0.9019 0.4229 0.2683 0.075 Uiso 1 1 calc R . .
C11 C 0.7505(4) 0.4568(4) 0.30406(8) 0.0445(13) Uani 1 1 d . . .
H11A H 0.8108 0.4812 0.2974 0.067 Uiso 1 1 calc R . .
H11B H 0.7603 0.4559 0.3179 0.067 Uiso 1 1 calc R . .
H11C H 0.7239 0.4972 0.3013 0.067 Uiso 1 1 calc R . .
C12 C 0.4573(6) 0.7419(6) 0.13309(11) 0.087(3) Uani 1 1 d . . .
H12A H 0.4979 0.7215 0.1271 0.131 Uiso 1 1 calc R . .
H12B H 0.4587 0.7357 0.1470 0.131 Uiso 1 1 calc R . .
H12C H 0.4797 0.8077 0.1298 0.131 Uiso 1 1 calc R . .
C13 C 0.2263(3) 0.5225(3) 0.07270(8) 0.0377(12) Uani 1 1 d . . .
H13A H 0.2368 0.4904 0.0618 0.045 Uiso 1 1 calc R . .
H13B H 0.2358 0.4952 0.0845 0.045 Uiso 1 1 calc R . .
C14 C 0.0246(5) 0.3585(4) 0.06944(14) 0.088(3) Uani 1 1 d . . .
H14A H 0.0375 0.3286 0.0802 0.132 Uiso 1 1 calc R . .
H14B H 0.0411 0.3395 0.0574 0.132 Uiso 1 1 calc R . .
H14C H -0.0423 0.3391 0.0693 0.132 Uiso 1 1 calc R . .
C15 C 0.0753(4) 0.5487(4) 0.05076(8) 0.0481(14) Uani 1 1 d . . .
H15A H 0.0094 0.5329 0.0507 0.072 Uiso 1 1 calc R . .
H15B H 0.0894 0.5262 0.0389 0.072 Uiso 1 1 calc R . .
H15C H 0.1159 0.6170 0.0517 0.072 Uiso 1 1 calc R . .
C16 C 0.0644(5) 0.5289(6) 0.09509(10) 0.076(2) Uani 1 1 d . . .
H16A H 0.1005 0.5975 0.0961 0.113 Uiso 1 1 calc R . .
H16B H 0.0788 0.5009 0.1060 0.113 Uiso 1 1 calc R . .
H16C H -0.0028 0.5078 0.0950 0.113 Uiso 1 1 calc R . .
C17 C 0.3333 0.6667 0.98001(12) 0.0301(18) Uani 1 3 d S . .
C18 C 0.4111(4) 0.7907(4) 0.94296(8) 0.0490(15) Uani 1 1 d . . .
H18A H 0.3826 0.8292 0.9459 0.073 Uiso 1 1 calc R . .
H18B H 0.4172 0.7876 0.9291 0.073 Uiso 1 1 calc R . .
H18C H 0.4734 0.8188 0.9489 0.073 Uiso 1 1 calc R . .
C19 C 0.2380(3) 0.5216(3) 1.01148(7) 0.0317(10) Uani 1 1 d . . .
H19A H 0.2447 0.5120 1.0253 0.038 Uiso 1 1 calc R . .
H19B H 0.1739 0.5118 1.0098 0.038 Uiso 1 1 calc R . .
C20 C 0.3658(4) 0.4498(4) 0.99276(8) 0.0493(14) Uani 1 1 d . . .
H20A H 0.3972 0.5060 0.9847 0.074 Uiso 1 1 calc R . .
H20B H 0.3637 0.3965 0.9860 0.074 Uiso 1 1 calc R . .
H20C H 0.4006 0.4608 1.0048 0.074 Uiso 1 1 calc R . .
C21 C 0.1711(4) 0.3979(4) 0.97518(8) 0.0506(15) Uani 1 1 d . . .
H21A H 0.1041 0.3681 0.9782 0.076 Uiso 1 1 calc R . .
H21B H 0.1823 0.3559 0.9671 0.076 Uiso 1 1 calc R . .
H21C H 0.1909 0.4571 0.9684 0.076 Uiso 1 1 calc R . .
C22 C 0.1836(5) 0.3131(4) 1.01384(9) 0.0614(19) Uani 1 1 d . . .
H22A H 0.2174 0.3260 1.0260 0.092 Uiso 1 1 calc R . .
H22B H 0.1856 0.2615 1.0072 0.092 Uiso 1 1 calc R . .
H22C H 0.1181 0.2954 1.0163 0.092 Uiso 1 1 calc R . .
O1 O 0.6667 0.3333 0.21800(8) 0.0285(12) Uani 1 3 d S . .
O2 O 0.6667 0.3333 0.27150(8) 0.0301(13) Uani 1 3 d S . .
O3 O 0.3333 0.6667 0.04635(9) 0.0364(14) Uani 1 3 d S . .
O4 O 0.3333 0.6667 0.09970(10) 0.0464(16) Uani 1 3 d S . .
Si1 Si 0.6667 0.3333 0.12747(4) 0.0441(7) Uani 1 3 d S . .
Si2 Si 0.89243(10) 0.53831(10) 0.17449(2) 0.0353(3) Uani 1 1 d . . .
Si3 Si 0.86368(10) 0.30323(10) 0.244273(19) 0.0292(3) Uani 1 1 d . . .
Si4 Si 0.6667 0.3333 0.29544(3) 0.0278(5) Uani 1 3 d S . .
Si5 Si 0.3333 0.6667 0.12420(5) 0.0587(8) Uani 1 3 d S . .
Si6 Si 0.09711(11) 0.49092(11) 0.07204(3) 0.0440(4) Uani 1 1 d . . .
Si7 Si 0.3333 0.6667 0.95285(3) 0.0305(5) Uani 1 3 d S . .
Si8 Si 0.24109(11) 0.42264(10) 0.99821(2) 0.0349(3) Uani 1 1 d . . .
W1 W 0.6667 0.3333 0.180397(4) 0.02536(8) Uani 1 3 d S . .
W2 W 0.6667 0.3333 0.243456(4) 0.02062(8) Uani 1 3 d S . .
W3 W 0.3333 0.6667 0.071724(5) 0.03068(9) Uani 1 3 d S . .
W4 W 0.3333 0.6667 1.005619(5) 0.02320(8) Uani 1 3 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.035(3) 0.035(3) 0.032(4) 0.000 0.000 0.0176(16)
C2 0.078(5) 0.069(5) 0.039(3) 0.018(3) 0.001(3) 0.039(4)
C3 0.038(3) 0.028(3) 0.035(3) 0.0014(19) 0.004(2) 0.016(2)
C4 0.061(4) 0.049(4) 0.042(3) 0.018(3) 0.014(3) 0.029(3)
C5 0.051(4) 0.060(4) 0.064(4) 0.015(3) 0.020(3) 0.036(3)
C6 0.048(4) 0.041(4) 0.067(4) 0.006(3) -0.003(3) 0.012(3)
C7 0.031(3) 0.027(2) 0.031(2) -0.0012(18) -0.0019(18) 0.016(2)
C8 0.040(3) 0.059(4) 0.045(3) 0.012(3) 0.011(2) 0.021(3)
C9 0.046(4) 0.052(4) 0.106(6) 0.009(4) 0.011(3) 0.033(3)
C10 0.035(3) 0.064(4) 0.040(3) -0.006(3) -0.007(2) 0.016(3)
C11 0.046(3) 0.042(3) 0.040(3) -0.007(2) -0.005(2) 0.017(3)
C12 0.082(6) 0.095(7) 0.077(5) -0.012(5) -0.027(4) 0.039(5)
C13 0.028(3) 0.028(3) 0.055(3) 0.000(2) -0.003(2) 0.013(2)
C14 0.034(4) 0.029(4) 0.184(9) 0.019(4) -0.015(4) 0.003(3)
C15 0.033(3) 0.047(4) 0.063(4) 0.003(3) -0.002(2) 0.019(3)
C16 0.054(4) 0.098(6) 0.076(5) 0.019(4) 0.019(4) 0.038(4)
C17 0.030(3) 0.030(3) 0.030(4) 0.000 0.000 0.0152(14)
C18 0.050(4) 0.042(3) 0.046(3) 0.014(2) 0.011(3) 0.016(3)
C19 0.029(3) 0.026(3) 0.037(3) 0.0021(19) 0.0016(19) 0.011(2)
C20 0.053(4) 0.053(4) 0.057(4) -0.008(3) -0.004(3) 0.038(3)
C21 0.061(4) 0.040(3) 0.038(3) -0.002(2) -0.011(3) 0.015(3)
C22 0.090(5) 0.030(3) 0.050(4) 0.004(3) -0.007(3) 0.020(3)
O1 0.030(2) 0.030(2) 0.025(3) 0.000 0.000 0.0151(10)
O2 0.031(2) 0.031(2) 0.029(3) 0.000 0.000 0.0153(10)
O3 0.027(2) 0.027(2) 0.056(4) 0.000 0.000 0.0133(10)
O4 0.044(3) 0.044(3) 0.051(4) 0.000 0.000 0.0220(13)
Si1 0.0534(11) 0.0534(11) 0.0255(12) 0.000 0.000 0.0267(5)
Si2 0.0315(8) 0.0306(8) 0.0401(8) 0.0097(6) 0.0065(6) 0.0127(7)
Si3 0.0254(7) 0.0334(8) 0.0320(7) 0.0012(5) 0.0008(5) 0.0171(6)
Si4 0.0291(8) 0.0291(8) 0.0253(11) 0.000 0.000 0.0145(4)
Si5 0.0636(14) 0.0636(14) 0.0489(18) 0.000 0.000 0.0318(7)
Si6 0.0243(8) 0.0329(8) 0.0685(11) 0.0101(7) 0.0046(7) 0.0095(7)
Si7 0.0311(8) 0.0311(8) 0.0292(11) 0.000 0.000 0.0156(4)
Si8 0.0435(9) 0.0234(7) 0.0344(7) -0.0001(5) -0.0021(6) 0.0141(7)
W1 0.02468(12) 0.02468(12) 0.02672(17) 0.000 0.000 0.01234(6)
W2 0.01949(11) 0.01949(11) 0.02289(15) 0.000 0.000 0.00975(5)
W3 0.02265(12) 0.02265(12) 0.0467(2) 0.000 0.000 0.01132(6)
W4 0.01975(11) 0.01975(11) 0.03010(17) 0.000 0.000 0.00988(6)

_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
C1 W1 1.796(8) . ?
C1 Si1 1.824(8) . ?
C2 Si1 1.874(6) . ?
C3 Si2 1.869(5) . ?
C3 W1 2.101(5) . ?
C4 Si2 1.864(5) . ?
C5 Si2 1.853(6) . ?
C6 Si2 1.873(6) . ?
C7 Si3 1.896(5) . ?
C7 W2 2.100(4) . ?
C8 Si3 1.859(5) . ?
C9 Si3 1.860(6) . ?
C10 Si3 1.866(5) . ?
C11 Si4 1.855(5) . ?
C12 Si5 1.845(7) . ?
C13 Si6 1.880(5) . ?
C13 W3 2.089(5) . ?
C14 Si6 1.858(6) . ?
C15 Si6 1.853(6) . ?
C16 Si6 1.859(7) . ?
C17 W4 1.752(8) . ?
C17 Si7 1.857(8) . ?
C18 Si7 1.875(5) . ?
C19 Si8 1.857(5) . ?
C19 W4 2.096(5) . ?
C20 Si8 1.867(6) . ?
C21 Si8 1.861(5) . ?
C22 Si8 1.865(6) . ?
O1 W2 1.741(5) . ?
O1 W1 2.572(5) . ?
O2 Si4 1.638(6) . ?
O2 W2 1.918(5) . ?
O3 W3 1.735(6) . ?
O4 Si5 1.675(7) . ?
O4 W3 1.913(7) . ?
Si1 C2 1.874(6) 3_665 ?
Si1 C2 1.874(6) 2_655 ?
Si4 C11 1.855(5) 3_665 ?
Si4 C11 1.855(5) 2_655 ?
Si5 C12 1.845(7) 2_665 ?
Si5 C12 1.845(7) 3_565 ?
Si7 C18 1.875(5) 2_665 ?
Si7 C18 1.875(5) 3_565 ?
W1 C3 2.101(5) 3_665 ?
W1 C3 2.101(5) 2_655 ?
W2 C7 2.100(4) 2_655 ?
W2 C7 2.100(4) 3_665 ?
W3 C13 2.089(5) 3_565 ?
W3 C13 2.089(5) 2_665 ?
W4 C19 2.096(5) 3_565 ?
W4 C19 2.096(5) 2_665 ?

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
W1 C1 Si1 180.0 . . ?
Si2 C3 W1 123.8(2) . . ?
Si3 C7 W2 118.9(2) . . ?
Si6 C13 W3 119.1(3) . . ?
W4 C17 Si7 180.000(1) . . ?
Si8 C19 W4 123.0(2) . . ?
W2 O1 W1 180.0 . . ?
Si4 O2 W2 180.0 . . ?
Si5 O4 W3 180.000(1) . . ?
C1 Si1 C2 110.0(2) . 3_665 ?
C1 Si1 C2 110.0(2) . 2_655 ?
C2 Si1 C2 108.9(2) 3_665 2_655 ?
C1 Si1 C2 110.0(2) . . ?
C2 Si1 C2 108.9(2) 3_665 . ?
C2 Si1 C2 108.9(2) 2_655 . ?
C5 Si2 C4 107.7(3) . . ?
C5 Si2 C3 114.3(3) . . ?
C4 Si2 C3 108.8(3) . . ?
C5 Si2 C6 108.1(3) . . ?
C4 Si2 C6 110.7(3) . . ?
C3 Si2 C6 107.2(3) . . ?
C8 Si3 C9 109.7(3) . . ?
C8 Si3 C10 109.3(3) . . ?
C9 Si3 C10 109.3(3) . . ?
C8 Si3 C7 110.7(2) . . ?
C9 Si3 C7 106.7(3) . . ?
C10 Si3 C7 111.2(2) . . ?
O2 Si4 C11 108.52(18) . 3_665 ?
O2 Si4 C11 108.52(18) . . ?
C11 Si4 C11 110.41(17) 3_665 . ?
O2 Si4 C11 108.52(18) . 2_655 ?
C11 Si4 C11 110.41(17) 3_665 2_655 ?
C11 Si4 C11 110.41(17) . 2_655 ?
O4 Si5 C12 109.2(3) . 2_665 ?
O4 Si5 C12 109.2(3) . . ?
C12 Si5 C12 109.7(3) 2_665 . ?
O4 Si5 C12 109.2(3) . 3_565 ?
C12 Si5 C12 109.7(3) 2_665 3_565 ?
C12 Si5 C12 109.7(3) . 3_565 ?
C16 Si6 C15 110.2(3) . . ?
C16 Si6 C14 109.9(4) . . ?
C15 Si6 C14 109.5(3) . . ?
C16 Si6 C13 110.4(3) . . ?
C15 Si6 C13 110.2(2) . . ?
C14 Si6 C13 106.8(3) . . ?
C17 Si7 C18 111.15(19) . 2_665 ?
C17 Si7 C18 111.2(2) . . ?
C18 Si7 C18 107.7(2) 2_665 . ?
C17 Si7 C18 111.15(19) . 3_565 ?
C18 Si7 C18 107.7(2) 2_665 3_565 ?
C18 Si7 C18 107.7(2) . 3_565 ?
C19 Si8 C21 108.9(3) . . ?
C19 Si8 C20 112.6(3) . . ?
C21 Si8 C20 110.3(3) . . ?
C19 Si8 C22 108.5(3) . . ?
C21 Si8 C22 108.8(3) . . ?
C20 Si8 C22 107.7(3) . . ?
C1 W1 C3 100.41(13) . 3_665 ?
C1 W1 C3 100.41(13) . . ?
C3 W1 C3 116.81(8) 3_665 . ?
C1 W1 C3 100.41(13) . 2_655 ?
C3 W1 C3 116.81(8) 3_665 2_655 ?
C3 W1 C3 116.81(8) . 2_655 ?
C1 W1 O1 180.000(1) . . ?
C3 W1 O1 79.59(13) 3_665 . ?
C3 W1 O1 79.59(13) . . ?
C3 W1 O1 79.59(13) 2_655 . ?
O1 W2 O2 180.000(1) . . ?
O1 W2 C7 92.38(12) . . ?
O2 W2 C7 87.62(12) . . ?
O1 W2 C7 92.38(12) . 2_655 ?
O2 W2 C7 87.62(12) . 2_655 ?
C7 W2 C7 119.830(19) . 2_655 ?
O1 W2 C7 92.38(12) . 3_665 ?
O2 W2 C7 87.62(12) . 3_665 ?
C7 W2 C7 119.830(18) . 3_665 ?
C7 W2 C7 119.830(18) 2_655 3_665 ?
O3 W3 O4 180.000(1) . . ?
O3 W3 C13 91.83(15) . 3_565 ?
O4 W3 C13 88.17(15) . 3_565 ?
O3 W3 C13 91.83(15) . . ?
O4 W3 C13 88.17(15) . . ?
C13 W3 C13 119.899(17) 3_565 . ?
O3 W3 C13 91.83(15) . 2_665 ?
O4 W3 C13 88.17(15) . 2_665 ?
C13 W3 C13 119.899(18) 3_565 2_665 ?
C13 W3 C13 119.899(17) . 2_665 ?
C17 W4 C19 101.03(13) . 3_565 ?
C17 W4 C19 101.03(13) . . ?
C19 W4 C19 116.43(8) 3_565 . ?
C17 W4 C19 101.03(13) . 2_665 ?
C19 W4 C19 116.43(8) 3_565 2_665 ?
C19 W4 C19 116.43(8) . 2_665 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W1 C1 Si1 C2 14(100) . . . 3_665 ?
W1 C1 Si1 C2 134(100) . . . 2_655 ?
W1 C1 Si1 C2 -106(100) . . . . ?
W1 C3 Si2 C5 -30.2(4) . . . . ?
W1 C3 Si2 C4 90.3(3) . . . . ?
W1 C3 Si2 C6 -150.0(3) . . . . ?
W2 C7 Si3 C8 -54.0(3) . . . . ?
W2 C7 Si3 C9 -173.3(3) . . . . ?
W2 C7 Si3 C10 67.6(3) . . . . ?
W2 O2 Si4 C11 143(100) . . . 3_665 ?
W2 O2 Si4 C11 -97(100) . . . . ?
W2 O2 Si4 C11 23(100) . . . 2_655 ?
W3 O4 Si5 C12 67(100) . . . 2_665 ?
W3 O4 Si5 C12 -53(100) . . . . ?
W3 O4 Si5 C12 -173(100) . . . 3_565 ?
W3 C13 Si6 C16 -68.8(4) . . . . ?
W3 C13 Si6 C15 53.0(4) . . . . ?
W3 C13 Si6 C14 171.8(4) . . . . ?
W4 C17 Si7 C18 68(100) . . . 2_665 ?
W4 C17 Si7 C18 -172(100) . . . . ?
W4 C17 Si7 C18 -52(100) . . . 3_565 ?
W4 C19 Si8 C21 -84.8(4) . . . . ?
W4 C19 Si8 C20 37.9(4) . . . . ?
W4 C19 Si8 C22 156.9(3) . . . . ?
Si1 C1 W1 C3 -72(100) . . . 3_665 ?
Si1 C1 W1 C3 48(100) . . . . ?
Si1 C1 W1 C3 168(100) . . . 2_655 ?
Si1 C1 W1 O1 0(45) . . . . ?
Si2 C3 W1 C1 -50.5(3) . . . . ?
Si2 C3 W1 C3 56.9(5) . . . 3_665 ?
Si2 C3 W1 C3 -157.9(2) . . . 2_655 ?
Si2 C3 W1 O1 129.5(3) . . . . ?
W2 O1 W1 C1 0(62) . . . . ?
W2 O1 W1 C3 -45(100) . . . 3_665 ?
W2 O1 W1 C3 -165(100) . . . . ?
W2 O1 W1 C3 75(100) . . . 2_655 ?
W1 O1 W2 O2 0(55) . . . . ?
W1 O1 W2 C7 54(100) . . . . ?
W1 O1 W2 C7 174(100) . . . 2_655 ?
W1 O1 W2 C7 -66(100) . . . 3_665 ?
Si4 O2 W2 O1 0(38) . . . . ?
Si4 O2 W2 C7 -149(100) . . . . ?
Si4 O2 W2 C7 91(100) . . . 2_655 ?
Si4 O2 W2 C7 -29(100) . . . 3_665 ?
Si3 C7 W2 O1 87.6(2) . . . . ?
Si3 C7 W2 O2 -92.4(2) . . . . ?
Si3 C7 W2 C7 -6.5(4) . . . 2_655 ?
Si3 C7 W2 C7 -178.28(5) . . . 3_665 ?
Si5 O4 W3 O3 0(25) . . . . ?
Si5 O4 W3 C13 -44(100) . . . 3_565 ?
Si5 O4 W3 C13 -164(100) . . . . ?
Si5 O4 W3 C13 76(100) . . . 2_665 ?
Si6 C13 W3 O3 -87.4(3) . . . . ?
Si6 C13 W3 O4 92.6(3) . . . . ?
Si6 C13 W3 C13 5.7(5) . . . 3_565 ?
Si6 C13 W3 C13 179.42(7) . . . 2_665 ?
Si7 C17 W4 C19 -130(100) . . . 3_565 ?
Si7 C17 W4 C19 -10(100) . . . . ?
Si7 C17 W4 C19 110(100) . . . 2_665 ?
Si8 C19 W4 C17 43.9(3) . . . . ?
Si8 C19 W4 C19 152.2(2) . . . 3_565 ?
Si8 C19 W4 C19 -64.4(4) . . . 2_665 ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         3.421
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.138

_database_code_depnum_ccdc_archive 'CCDC 949735'