# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?
loop_
_publ_author_name
_publ_author_address
'Rudolf Pietschnig'
; Institute of Chemistry,
Karl-Franzens University Graz,
Schubertstr. 1,
A-8010 Graz,
Austria
;
'Ferdinand Belaj' ''
'Martin Nieger' ''
'Stefan Spirk' ''

_publ_contact_author_name        'Dr Rudolf Pietschnig'
_publ_contact_author_email       RUDOLF.PIETSCHNIG@UNI-GRAZ.AT

_publ_section_title              
;
Formation and Hydrogen Bonding of a Novel
POSS-Trisilanol
;
_publ_contact_author_address     
; Institute of Chemistry,
Karl-Franzens University Graz,
Schubertstr. 1,
A-8010 Graz,
Austria
;
_publ_contact_author_fax         43(316)3809835
_publ_contact_author_phone       43(316)3805287
_publ_requested_category         FO

#==============================================================================
# End of Crystallographic Information File

# Attachment '5.cif'

data_stsce2
_database_code_depnum_ccdc_archive 'CCDC 681704'

_audit_creation_method           'manual edited SHELXL-97 .cif file'
_chemical_compound_source        'synthetical product'

_chemical_name_systematic        
; 1,3-Di(tert-butyl)-1,1,3,3-tetrahydroxydisiloxane
;
_chemical_name_common            
1,3-Di(tert-butyl)-1,1,3,3-tetrahydroxydisiloxane
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H22 O5 Si2'
_chemical_formula_sum            'C8 H22 O5 Si2'
_chemical_formula_weight         254.44

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.222(2)
_cell_length_b                   9.674(3)
_cell_length_c                   11.948(3)
_cell_angle_alpha                89.11(3)
_cell_angle_beta                 79.67(3)
_cell_angle_gamma                81.70(3)
_cell_volume                     700.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    95(2)
_cell_measurement_reflns_used    32
_cell_measurement_theta_min      15.07
_cell_measurement_theta_max      17.71

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             276
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      95(2)
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  Stoe
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_wavelength     0.71069
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            3314
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0787
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.73
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2736
_reflns_number_gt                1841
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'local software'
_computing_cell_refinement       'local software'
_computing_data_reduction        'local software'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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.

The non-hydrogen atoms were refined with anisotropic displacement parameters
without any constraints.

The H atoms of the methyl groups were refined with common isotropic
displacement parameters for the H atoms of the same group and idealized
geometry with tetrahedral angles, enabling rotation around the X-C bond,
and C-H distances of 0.98 \%A (AFIX 137 of SHELXL-97).

The H atoms of the OH groups are disordered over two sites. They were refined
with site occupation factors of 0.5 and with a common isotropic displacement
parameter. The bond length was fixed to be 0.84 \%A.
;

_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^)+(0.0770P)^2^+0.0336P] 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    refU
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2736
_refine_ls_number_parameters     174
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0623
_refine_ls_wR_factor_ref         0.1649
_refine_ls_wR_factor_gt          0.1449
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.7623(4) 0.5255(3) 0.2458(2) 0.0249(6) Uani 1 1 d . . .
Si1 Si 0.62657(14) 0.57745(10) 0.14628(8) 0.0177(3) Uani 1 1 d D . .
O2 O 0.7801(3) 0.5288(3) 0.0232(2) 0.0255(6) Uani 1 1 d D . .
H22 H 0.9179(8) 0.524(8) 0.015(2) 0.028(8) Uiso 0.50 1 d PD . .
H23 H 0.720(3) 0.508(7) -0.0304(19) 0.028(8) Uiso 0.50 1 d PD . .
O3 O 0.4093(3) 0.4983(3) 0.1572(2) 0.0256(6) Uani 1 1 d D . .
H32 H 0.356(6) 0.485(6) 0.0991(11) 0.028(8) Uiso 0.50 1 d PD . .
H35 H 0.300(4) 0.522(5) 0.209(3) 0.028(8) Uiso 0.50 1 d PD . .
C1 C 0.5473(6) 0.7706(4) 0.1563(3) 0.0299(9) Uani 1 1 d . . .
C11 C 0.4133(7) 0.8177(4) 0.0623(4) 0.0396(11) Uani 1 1 d . . .
H111 H 0.2811 0.7714 0.0723 0.051(8) Uiso 1 1 calc R . .
H112 H 0.5041 0.7924 -0.0123 0.051(8) Uiso 1 1 calc R . .
H113 H 0.3695 0.9192 0.0671 0.051(8) Uiso 1 1 calc R . .
C12 C 0.7540(7) 0.8416(4) 0.1403(4) 0.0415(11) Uani 1 1 d . . .
H121 H 0.8471 0.8131 0.0669 0.050(8) Uiso 1 1 calc R . .
H122 H 0.8364 0.8142 0.2017 0.050(8) Uiso 1 1 calc R . .
H123 H 0.7114 0.9433 0.1421 0.050(8) Uiso 1 1 calc R . .
C13 C 0.4054(7) 0.8100(4) 0.2731(4) 0.0426(11) Uani 1 1 d . . .
H131 H 0.3644 0.9116 0.2787 0.057(9) Uiso 1 1 calc R . .
H132 H 0.4895 0.7780 0.3329 0.057(9) Uiso 1 1 calc R . .
H133 H 0.2716 0.7654 0.2824 0.057(9) Uiso 1 1 calc R . .
Si2 Si 0.86473(14) 0.44043(10) 0.34596(8) 0.0183(3) Uani 1 1 d D . .
O4 O 0.7183(3) 0.4949(3) 0.46827(19) 0.0256(6) Uani 1 1 d D . .
H44 H 0.582(2) 0.493(7) 0.482(3) 0.028(8) Uiso 0.50 1 d PD . .
H45 H 0.778(3) 0.496(7) 0.5259(15) 0.028(8) Uiso 0.50 1 d PD . .
O5 O 1.1082(3) 0.4833(3) 0.3449(2) 0.0261(6) Uani 1 1 d D . .
H53 H 1.206(4) 0.471(7) 0.2862(19) 0.028(8) Uiso 0.50 1 d PD . .
H54 H 1.158(5) 0.486(8) 0.4055(11) 0.028(8) Uiso 0.50 1 d PD . .
C2 C 0.8761(6) 0.2493(4) 0.3257(3) 0.0272(8) Uani 1 1 d . . .
C21 C 1.0064(7) 0.2046(4) 0.2066(4) 0.0410(11) Uani 1 1 d . . .
H211 H 1.1572 0.2265 0.1993 0.051(8) Uiso 1 1 calc R . .
H212 H 0.9338 0.2550 0.1486 0.051(8) Uiso 1 1 calc R . .
H213 H 1.0110 0.1039 0.1962 0.051(8) Uiso 1 1 calc R . .
C22 C 0.9918(7) 0.1712(4) 0.4164(4) 0.0407(11) Uani 1 1 d . . .
H221 H 0.9931 0.0705 0.4078 0.039(7) Uiso 1 1 calc R . .
H222 H 0.9122 0.2019 0.4923 0.039(7) Uiso 1 1 calc R . .
H223 H 1.1438 0.1914 0.4070 0.039(7) Uiso 1 1 calc R . .
C23 C 0.6424(7) 0.2125(4) 0.3379(4) 0.0405(11) Uani 1 1 d . . .
H231 H 0.6497 0.1118 0.3263 0.077(11) Uiso 1 1 calc R . .
H232 H 0.5671 0.2631 0.2809 0.077(11) Uiso 1 1 calc R . .
H233 H 0.5605 0.2390 0.4142 0.077(11) Uiso 1 1 calc R . .

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
O1 0.0232(13) 0.0365(15) 0.0167(13) 0.0008(11) -0.0100(10) -0.0026(11)
Si1 0.0100(4) 0.0285(5) 0.0150(5) 0.0006(4) -0.0042(4) -0.0017(4)
O2 0.0140(12) 0.0422(15) 0.0198(14) -0.0057(12) -0.0040(10) -0.0009(11)
O3 0.0160(12) 0.0418(15) 0.0207(14) -0.0006(12) -0.0049(11) -0.0083(11)
C1 0.028(2) 0.032(2) 0.027(2) -0.0011(17) -0.0036(17) 0.0023(16)
C11 0.030(2) 0.038(2) 0.049(3) 0.009(2) -0.009(2) 0.0048(17)
C12 0.041(2) 0.039(2) 0.047(3) -0.003(2) -0.007(2) -0.0143(19)
C13 0.036(2) 0.040(2) 0.045(3) -0.009(2) 0.005(2) 0.0036(19)
Si2 0.0098(4) 0.0310(5) 0.0147(5) 0.0006(4) -0.0042(4) -0.0020(4)
O4 0.0145(12) 0.0447(15) 0.0172(13) -0.0030(12) -0.0039(10) -0.0010(11)
O5 0.0151(12) 0.0463(16) 0.0175(14) -0.0009(13) -0.0046(10) -0.0046(11)
C2 0.0226(18) 0.0279(19) 0.030(2) 0.0029(16) -0.0035(16) -0.0019(14)
C21 0.043(2) 0.039(2) 0.035(3) -0.011(2) 0.005(2) 0.0007(19)
C22 0.033(2) 0.039(2) 0.044(3) 0.014(2) -0.002(2) 0.0068(18)
C23 0.031(2) 0.036(2) 0.054(3) -0.005(2) 0.001(2) -0.0122(17)

_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
O1 Si1 1.612(2) . yes
O1 Si2 1.614(2) . yes
Si1 O3 1.632(2) . yes
Si1 O2 1.638(3) . yes
Si1 C1 1.862(4) . yes
O2 H22 0.84 . ?
O2 H23 0.84 . ?
O3 H32 0.84 . ?
O3 H35 0.84 . ?
C1 C12 1.525(5) . ?
C1 C13 1.533(6) . ?
C1 C11 1.541(5) . ?
C11 H111 0.98 . ?
C11 H112 0.98 . ?
C11 H113 0.98 . ?
C12 H121 0.98 . ?
C12 H122 0.98 . ?
C12 H123 0.98 . ?
C13 H131 0.98 . ?
C13 H132 0.98 . ?
C13 H133 0.98 . ?
Si2 O5 1.625(2) . yes
Si2 O4 1.628(2) . yes
Si2 C2 1.858(4) . yes
O4 H44 0.84 . ?
O4 H45 0.84 . ?
O5 H53 0.84 . ?
O5 H54 0.84 . ?
C2 C23 1.528(5) . ?
C2 C22 1.536(5) . ?
C2 C21 1.540(6) . ?
C21 H211 0.98 . ?
C21 H212 0.98 . ?
C21 H213 0.98 . ?
C22 H221 0.98 . ?
C22 H222 0.98 . ?
C22 H223 0.98 . ?
C23 H231 0.98 . ?
C23 H232 0.98 . ?
C23 H233 0.98 . ?

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 O1 Si2 165.56(18) . . yes
O1 Si1 O3 109.57(14) . . yes
O1 Si1 O2 108.73(13) . . yes
O3 Si1 O2 106.11(13) . . yes
O1 Si1 C1 109.51(16) . . yes
O3 Si1 C1 111.14(16) . . yes
O2 Si1 C1 111.69(17) . . yes
Si1 O2 H22 119.4(11) . . ?
Si1 O2 H23 119.4(11) . . ?
H22 O2 H23 121(2) . . ?
Si1 O3 H32 120.0(11) . . ?
Si1 O3 H35 119.9(11) . . ?
H32 O3 H35 105(4) . . ?
C12 C1 C13 109.8(4) . . ?
C12 C1 C11 109.6(3) . . ?
C13 C1 C11 109.5(3) . . ?
C12 C1 Si1 109.9(3) . . ?
C13 C1 Si1 109.4(3) . . ?
C11 C1 Si1 108.7(3) . . ?
C1 C11 H111 109.5 . . ?
C1 C11 H112 109.5 . . ?
H111 C11 H112 109.5 . . ?
C1 C11 H113 109.5 . . ?
H111 C11 H113 109.5 . . ?
H112 C11 H113 109.5 . . ?
C1 C12 H121 109.5 . . ?
C1 C12 H122 109.5 . . ?
H121 C12 H122 109.5 . . ?
C1 C12 H123 109.5 . . ?
H121 C12 H123 109.5 . . ?
H122 C12 H123 109.5 . . ?
C1 C13 H131 109.5 . . ?
C1 C13 H132 109.5 . . ?
H131 C13 H132 109.5 . . ?
C1 C13 H133 109.5 . . ?
H131 C13 H133 109.5 . . ?
H132 C13 H133 109.5 . . ?
O1 Si2 O5 107.69(14) . . yes
O1 Si2 O4 108.95(13) . . yes
O5 Si2 O4 105.61(13) . . yes
O1 Si2 C2 110.59(16) . . yes
O5 Si2 C2 111.85(15) . . yes
O4 Si2 C2 111.92(17) . . yes
Si2 O4 H44 120.3(11) . . ?
Si2 O4 H45 120.3(11) . . ?
H44 O4 H45 115(3) . . ?
Si2 O5 H53 120.6(11) . . ?
Si2 O5 H54 120.6(11) . . ?
H53 O5 H54 114(3) . . ?
C23 C2 C22 109.1(3) . . ?
C23 C2 C21 109.4(3) . . ?
C22 C2 C21 109.3(3) . . ?
C23 C2 Si2 109.9(3) . . ?
C22 C2 Si2 109.2(3) . . ?
C21 C2 Si2 109.8(3) . . ?
C2 C21 H211 109.5 . . ?
C2 C21 H212 109.5 . . ?
H211 C21 H212 109.5 . . ?
C2 C21 H213 109.5 . . ?
H211 C21 H213 109.5 . . ?
H212 C21 H213 109.5 . . ?
C2 C22 H221 109.5 . . ?
C2 C22 H222 109.5 . . ?
H221 C22 H222 109.5 . . ?
C2 C22 H223 109.5 . . ?
H221 C22 H223 109.5 . . ?
H222 C22 H223 109.5 . . ?
C2 C23 H231 109.5 . . ?
C2 C23 H232 109.5 . . ?
H231 C23 H232 109.5 . . ?
C2 C23 H233 109.5 . . ?
H231 C23 H233 109.5 . . ?
H232 C23 H233 109.5 . . ?

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
Si2 O1 Si1 O3 20.9(8) . . . . yes
Si2 O1 Si1 O2 -94.7(8) . . . . ?
Si2 O1 Si1 C1 143.0(7) . . . . yes
O1 Si1 C1 C12 61.4(3) . . . . ?
O3 Si1 C1 C12 -177.4(3) . . . . yes
O2 Si1 C1 C12 -59.1(3) . . . . ?
O1 Si1 C1 C13 -59.2(3) . . . . ?
O3 Si1 C1 C13 62.0(3) . . . . ?
O2 Si1 C1 C13 -179.7(3) . . . . yes
O1 Si1 C1 C11 -178.7(3) . . . . yes
O3 Si1 C1 C11 -57.5(3) . . . . ?
O2 Si1 C1 C11 60.8(3) . . . . ?
Si1 O1 Si2 O5 152.8(7) . . . . yes
Si1 O1 Si2 O4 -93.1(8) . . . . ?
Si1 O1 Si2 C2 30.3(8) . . . . yes
O1 Si2 C2 C23 -65.0(3) . . . . ?
O5 Si2 C2 C23 175.0(3) . . . . yes
O4 Si2 C2 C23 56.7(3) . . . . ?
O1 Si2 C2 C22 175.3(2) . . . . yes
O5 Si2 C2 C22 55.3(3) . . . . ?
O4 Si2 C2 C22 -63.0(3) . . . . ?
O1 Si2 C2 C21 55.5(3) . . . . ?
O5 Si2 C2 C21 -64.6(3) . . . . ?
O4 Si2 C2 C21 177.1(2) . . . . yes

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H22 O2 0.84 1.850(13) 2.671(4) 165(5) 2_765
O2 H23 O3 0.84 1.843(16) 2.669(3) 167(7) 2_665
O3 H32 O2 0.84 1.831(6) 2.669(3) 175(6) 2_665
O3 H35 O5 0.84 1.90(3) 2.668(3) 151(6) 1_455
O4 H44 O4 0.84 1.841(5) 2.674(4) 171(2) 2_666
O4 H45 O5 0.84 1.835(7) 2.672(3) 174(6) 2_766
O5 H53 O3 0.84 1.852(19) 2.668(3) 163(6) 1_655
O5 H54 O4 0.84 1.835(5) 2.672(3) 174(4) 2_766

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.090


# Attachment '2and4.cif'

data_rp007_hy
_database_code_depnum_ccdc_archive 'CCDC 682320'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Hexa-ter.butyl-tetracyclo[5.5.1.1(3,11).1(5,9)]hexasiloxane
;
_chemical_name_common            
Hexa-ter.butyl-tetracyclo(5.5.1.1(3,11).1(5,9))hexasiloxane
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H54 O9 Si6'
_chemical_formula_sum            'C24 H54 O9 Si6'
_chemical_formula_weight         655.21

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   'P 21/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                   11.935(2)
_cell_length_b                   18.912(4)
_cell_length_c                   16.722(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.37(2)
_cell_angle_gamma                90.00
_cell_volume                     3602.3(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    37
_cell_measurement_theta_min      1
_cell_measurement_theta_max      25

_exptl_crystal_description       plates
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1416
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
dx = 40 mm, 160 sec./deg. 1 deg., 3 sets, 469 frames,
scaling using SADABS, T-ratio= 0.6166
;

_diffrn_ambient_temperature      123(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-Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi ane omage, 1 deg.'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32311
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         5.00
_diffrn_reflns_theta_max         25.03
_reflns_number_total             6295
_reflns_number_gt                4618
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Collect
_computing_cell_refinement       'DIRAX, EVALCCD'
_computing_data_reduction        EVALCCD
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.0377P)^2^+5.3259P] 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    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6295
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1134
_refine_ls_wR_factor_gt          0.1029
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.76194(7) 0.19917(4) 0.51939(5) 0.01330(19) Uani 1 1 d . . .
Si2 Si 0.71860(7) 0.34213(4) 0.44283(5) 0.01434(19) Uani 1 1 d . . .
Si3 Si 0.82707(7) 0.32762(4) 0.62631(5) 0.01385(19) Uani 1 1 d . . .
Si4 Si 0.52034(7) 0.19988(4) 0.54332(5) 0.01273(18) Uani 1 1 d . . .
Si5 Si 0.47419(7) 0.34290(4) 0.46796(5) 0.01372(19) Uani 1 1 d . . .
Si6 Si 0.58570(7) 0.32759(4) 0.65120(5) 0.01414(19) Uani 1 1 d . . .
O1 O 0.73678(17) 0.25607(9) 0.44218(12) 0.0157(4) Uani 1 1 d . . .
O2 O 0.79353(17) 0.36900(10) 0.53644(12) 0.0165(4) Uani 1 1 d . . .
O3 O 0.82666(17) 0.24322(9) 0.60496(12) 0.0151(4) Uani 1 1 d . . .
O4 O 0.45727(17) 0.25699(9) 0.47016(12) 0.0150(4) Uani 1 1 d . . .
O5 O 0.51336(17) 0.36936(10) 0.56571(12) 0.0161(4) Uani 1 1 d . . .
O6 O 0.56081(17) 0.24332(9) 0.63162(12) 0.0150(4) Uani 1 1 d . . .
O7 O 0.63696(17) 0.16861(9) 0.52463(12) 0.0163(4) Uani 1 1 d . . .
O8 O 0.58030(17) 0.35938(10) 0.42815(12) 0.0164(4) Uani 1 1 d . . .
O9 O 0.72513(17) 0.34284(10) 0.67063(13) 0.0171(4) Uani 1 1 d . . .
C11 C 0.8553(3) 0.12454(15) 0.50543(19) 0.0173(6) Uani 1 1 d . . .
C12 C 0.9722(3) 0.15322(18) 0.4989(2) 0.0314(8) Uani 1 1 d . . .
H12A H 1.0122 0.1794 0.5500 0.047 Uiso 1 1 calc R . .
H12B H 0.9575 0.1849 0.4505 0.047 Uiso 1 1 calc R . .
H12C H 1.0217 0.1138 0.4920 0.047 Uiso 1 1 calc R . .
C13 C 0.7922(3) 0.08321(17) 0.4252(2) 0.0271(8) Uani 1 1 d . . .
H13A H 0.7175 0.0648 0.4297 0.041 Uiso 1 1 calc R . .
H13B H 0.8417 0.0438 0.4183 0.041 Uiso 1 1 calc R . .
H13C H 0.7771 0.1148 0.3767 0.041 Uiso 1 1 calc R . .
C14 C 0.8786(3) 0.07487(17) 0.5812(2) 0.0289(8) Uani 1 1 d . . .
H14A H 0.9193 0.1009 0.6323 0.043 Uiso 1 1 calc R . .
H14B H 0.9275 0.0352 0.5739 0.043 Uiso 1 1 calc R . .
H14C H 0.8038 0.0568 0.5858 0.043 Uiso 1 1 calc R . .
C21 C 0.7690(3) 0.38673(15) 0.3610(2) 0.0208(7) Uani 1 1 d . . .
C22 C 0.7576(4) 0.46684(18) 0.3688(3) 0.0451(11) Uani 1 1 d . . .
H22A H 0.6753 0.4790 0.3615 0.068 Uiso 1 1 calc R . .
H22B H 0.7842 0.4905 0.3257 0.068 Uiso 1 1 calc R . .
H22C H 0.8059 0.4823 0.4244 0.068 Uiso 1 1 calc R . .
C23 C 0.6936(4) 0.3628(2) 0.2743(2) 0.0483(11) Uani 1 1 d . . .
H23A H 0.6111 0.3742 0.2673 0.072 Uiso 1 1 calc R . .
H23B H 0.7020 0.3117 0.2687 0.072 Uiso 1 1 calc R . .
H23C H 0.7194 0.3873 0.2312 0.072 Uiso 1 1 calc R . .
C24 C 0.8971(3) 0.3685(2) 0.3720(3) 0.0396(9) Uani 1 1 d . . .
H24A H 0.9455 0.3837 0.4276 0.059 Uiso 1 1 calc R . .
H24B H 0.9232 0.3928 0.3289 0.059 Uiso 1 1 calc R . .
H24C H 0.9050 0.3173 0.3664 0.059 Uiso 1 1 calc R . .
C31 C 0.9717(3) 0.35515(15) 0.6973(2) 0.0205(7) Uani 1 1 d . . .
C32 C 0.9692(3) 0.43508(17) 0.7160(2) 0.0342(9) Uani 1 1 d . . .
H32A H 0.9068 0.4448 0.7415 0.051 Uiso 1 1 calc R . .
H32B H 0.9544 0.4618 0.6636 0.051 Uiso 1 1 calc R . .
H32C H 1.0450 0.4493 0.7547 0.051 Uiso 1 1 calc R . .
C33 C 0.9959(3) 0.31332(19) 0.7791(2) 0.0334(8) Uani 1 1 d . . .
H33A H 0.9973 0.2626 0.7672 0.050 Uiso 1 1 calc R . .
H33B H 0.9339 0.3229 0.8051 0.050 Uiso 1 1 calc R . .
H33C H 1.0719 0.3276 0.8175 0.050 Uiso 1 1 calc R . .
C34 C 1.0681(3) 0.34017(19) 0.6566(2) 0.0328(8) Uani 1 1 d . . .
H34A H 1.0697 0.2895 0.6447 0.049 Uiso 1 1 calc R . .
H34B H 1.1442 0.3546 0.6947 0.049 Uiso 1 1 calc R . .
H34C H 1.0523 0.3669 0.6041 0.049 Uiso 1 1 calc R . .
C41 C 0.4201(3) 0.12640(15) 0.54903(19) 0.0185(7) Uani 1 1 d . . .
C42 C 0.3925(3) 0.08271(17) 0.4679(2) 0.0285(8) Uani 1 1 d . . .
H42A H 0.4657 0.0642 0.4609 0.043 Uiso 1 1 calc R . .
H42B H 0.3535 0.1128 0.4199 0.043 Uiso 1 1 calc R . .
H42C H 0.3407 0.0433 0.4710 0.043 Uiso 1 1 calc R . .
C43 C 0.3064(3) 0.15572(18) 0.5604(2) 0.0313(8) Uani 1 1 d . . .
H43A H 0.2671 0.1856 0.5123 0.047 Uiso 1 1 calc R . .
H43B H 0.3247 0.1839 0.6119 0.047 Uiso 1 1 calc R . .
H43C H 0.2547 0.1165 0.5642 0.047 Uiso 1 1 calc R . .
C44 C 0.4817(3) 0.07940(16) 0.6243(2) 0.0285(8) Uani 1 1 d . . .
H44A H 0.5546 0.0606 0.6171 0.043 Uiso 1 1 calc R . .
H44B H 0.4299 0.0401 0.6281 0.043 Uiso 1 1 calc R . .
H44C H 0.4999 0.1075 0.6759 0.043 Uiso 1 1 calc R . .
C51 C 0.3373(3) 0.38791(15) 0.4066(2) 0.0209(7) Uani 1 1 d . . .
C52 C 0.3563(3) 0.46842(16) 0.4163(2) 0.0340(9) Uani 1 1 d . . .
H52A H 0.4213 0.4822 0.3950 0.051 Uiso 1 1 calc R . .
H52B H 0.3753 0.4813 0.4756 0.051 Uiso 1 1 calc R . .
H52C H 0.2846 0.4930 0.3844 0.051 Uiso 1 1 calc R . .
C53 C 0.2359(3) 0.36643(18) 0.4400(2) 0.0307(8) Uani 1 1 d . . .
H53A H 0.2549 0.3794 0.4993 0.046 Uiso 1 1 calc R . .
H53B H 0.2237 0.3152 0.4340 0.046 Uiso 1 1 calc R . .
H53C H 0.1641 0.3909 0.4081 0.046 Uiso 1 1 calc R . .
C54 C 0.3089(3) 0.36777(19) 0.3138(2) 0.0307(8) Uani 1 1 d . . .
H54A H 0.3743 0.3816 0.2930 0.046 Uiso 1 1 calc R . .
H54B H 0.2373 0.3923 0.2815 0.046 Uiso 1 1 calc R . .
H54C H 0.2969 0.3166 0.3076 0.046 Uiso 1 1 calc R . .
C61 C 0.5388(3) 0.35241(16) 0.7433(2) 0.0218(7) Uani 1 1 d . . .
C62 C 0.5706(4) 0.42960(18) 0.7685(2) 0.0389(9) Uani 1 1 d . . .
H62A H 0.6556 0.4361 0.7808 0.058 Uiso 1 1 calc R . .
H62B H 0.5472 0.4410 0.8184 0.058 Uiso 1 1 calc R . .
H62C H 0.5295 0.4609 0.7224 0.058 Uiso 1 1 calc R . .
C63 C 0.6042(3) 0.30333(19) 0.8159(2) 0.0322(8) Uani 1 1 d . . .
H63A H 0.6890 0.3099 0.8278 0.048 Uiso 1 1 calc R . .
H63B H 0.5839 0.2540 0.8000 0.048 Uiso 1 1 calc R . .
H63C H 0.5812 0.3148 0.8659 0.048 Uiso 1 1 calc R . .
C64 C 0.4062(3) 0.34214(19) 0.7241(2) 0.0326(8) Uani 1 1 d . . .
H64A H 0.3858 0.2929 0.7077 0.049 Uiso 1 1 calc R . .
H64B H 0.3649 0.3736 0.6782 0.049 Uiso 1 1 calc R . .
H64C H 0.3828 0.3533 0.7741 0.049 Uiso 1 1 calc R . .

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
Si1 0.0140(4) 0.0127(4) 0.0124(4) 0.0003(3) 0.0028(3) 0.0008(3)
Si2 0.0151(4) 0.0144(4) 0.0127(4) 0.0015(3) 0.0031(3) -0.0009(3)
Si3 0.0127(4) 0.0143(4) 0.0126(4) -0.0012(3) 0.0008(3) -0.0015(3)
Si4 0.0136(4) 0.0119(4) 0.0116(4) 0.0001(3) 0.0021(3) -0.0014(3)
Si5 0.0129(4) 0.0130(4) 0.0134(4) 0.0012(3) 0.0009(3) 0.0007(3)
Si6 0.0145(4) 0.0155(4) 0.0118(4) -0.0026(3) 0.0030(3) -0.0003(3)
O1 0.0206(11) 0.0136(10) 0.0118(11) 0.0007(8) 0.0033(9) -0.0002(8)
O2 0.0181(11) 0.0152(10) 0.0147(11) 0.0009(8) 0.0025(9) -0.0010(8)
O3 0.0195(11) 0.0113(10) 0.0129(11) 0.0005(8) 0.0024(9) 0.0005(8)
O4 0.0176(11) 0.0126(10) 0.0129(11) -0.0001(8) 0.0018(9) -0.0008(8)
O5 0.0180(11) 0.0149(10) 0.0141(11) -0.0013(8) 0.0027(9) 0.0006(8)
O6 0.0167(11) 0.0155(10) 0.0119(11) -0.0011(8) 0.0028(9) -0.0018(8)
O7 0.0185(11) 0.0122(10) 0.0174(11) -0.0012(8) 0.0039(9) -0.0009(8)
O8 0.0168(11) 0.0170(10) 0.0134(11) 0.0045(8) 0.0014(9) 0.0013(8)
O9 0.0163(11) 0.0183(11) 0.0144(11) -0.0034(8) 0.0012(9) -0.0027(8)
C11 0.0188(16) 0.0171(15) 0.0163(16) 0.0003(12) 0.0056(13) 0.0053(12)
C12 0.0246(19) 0.034(2) 0.040(2) -0.0018(16) 0.0159(17) 0.0058(14)
C13 0.0309(19) 0.0263(18) 0.0234(19) -0.0062(14) 0.0069(16) 0.0078(14)
C14 0.037(2) 0.0249(18) 0.0242(19) 0.0071(14) 0.0079(16) 0.0104(14)
C21 0.0235(17) 0.0228(16) 0.0171(17) 0.0048(13) 0.0076(14) -0.0012(13)
C22 0.064(3) 0.027(2) 0.055(3) 0.0170(18) 0.035(2) 0.0010(18)
C23 0.057(3) 0.071(3) 0.017(2) 0.0101(19) 0.0107(19) -0.017(2)
C24 0.030(2) 0.054(2) 0.042(2) 0.0165(19) 0.0210(19) 0.0040(17)
C31 0.0186(16) 0.0202(16) 0.0189(17) -0.0025(13) -0.0003(13) -0.0027(12)
C32 0.030(2) 0.0251(18) 0.040(2) -0.0091(16) -0.0018(17) -0.0064(14)
C33 0.0279(19) 0.042(2) 0.0218(19) 0.0021(15) -0.0055(15) -0.0040(15)
C34 0.0170(18) 0.043(2) 0.036(2) -0.0046(16) 0.0044(16) -0.0058(15)
C41 0.0205(17) 0.0159(15) 0.0169(17) 0.0031(12) 0.0020(13) -0.0052(12)
C42 0.033(2) 0.0221(17) 0.0251(19) -0.0037(14) 0.0010(16) -0.0107(14)
C43 0.0211(18) 0.035(2) 0.038(2) 0.0042(16) 0.0106(16) -0.0070(14)
C44 0.034(2) 0.0203(17) 0.026(2) 0.0067(14) 0.0023(16) -0.0076(14)
C51 0.0159(16) 0.0200(16) 0.0212(18) 0.0007(13) -0.0031(13) 0.0021(12)
C52 0.030(2) 0.0184(17) 0.044(2) 0.0047(15) -0.0039(17) 0.0086(14)
C53 0.0164(17) 0.036(2) 0.037(2) -0.0012(16) 0.0033(16) 0.0032(14)
C54 0.0234(19) 0.040(2) 0.0211(19) 0.0041(15) -0.0046(15) 0.0021(15)
C61 0.0210(17) 0.0256(17) 0.0184(17) -0.0047(13) 0.0054(14) 0.0015(13)
C62 0.051(3) 0.033(2) 0.035(2) -0.0198(17) 0.0160(19) -0.0022(17)
C63 0.037(2) 0.045(2) 0.0142(18) -0.0003(15) 0.0075(16) 0.0037(16)
C64 0.0254(19) 0.047(2) 0.030(2) -0.0054(16) 0.0158(16) 0.0017(16)

_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
Si1 O7 1.626(2) . ?
Si1 O3 1.637(2) . ?
Si1 O1 1.638(2) . ?
Si1 C11 1.855(3) . ?
Si2 O8 1.628(2) . ?
Si2 O2 1.635(2) . ?
Si2 O1 1.642(2) . ?
Si2 C21 1.853(3) . ?
Si3 O9 1.628(2) . ?
Si3 O2 1.635(2) . ?
Si3 O3 1.635(2) . ?
Si3 C31 1.853(3) . ?
Si4 O7 1.626(2) . ?
Si4 O6 1.632(2) . ?
Si4 O4 1.637(2) . ?
Si4 C41 1.855(3) . ?
Si5 O8 1.627(2) . ?
Si5 O5 1.639(2) . ?
Si5 O4 1.6389(19) . ?
Si5 C51 1.856(3) . ?
Si6 O9 1.623(2) . ?
Si6 O5 1.636(2) . ?
Si6 O6 1.636(2) . ?
Si6 C61 1.849(3) . ?
C11 C12 1.532(4) . ?
C11 C14 1.535(4) . ?
C11 C13 1.541(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C21 C24 1.525(5) . ?
C21 C23 1.530(5) . ?
C21 C22 1.530(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C31 C34 1.529(5) . ?
C31 C33 1.531(4) . ?
C31 C32 1.546(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C41 C43 1.528(4) . ?
C41 C44 1.538(4) . ?
C41 C42 1.539(4) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C51 C53 1.532(5) . ?
C51 C54 1.534(4) . ?
C51 C52 1.541(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C61 C64 1.531(4) . ?
C61 C62 1.535(4) . ?
C61 C63 1.542(4) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?

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
O7 Si1 O3 109.56(11) . . ?
O7 Si1 O1 108.70(11) . . ?
O3 Si1 O1 106.40(10) . . ?
O7 Si1 C11 109.33(12) . . ?
O3 Si1 C11 110.67(12) . . ?
O1 Si1 C11 112.10(12) . . ?
O8 Si2 O2 108.80(11) . . ?
O8 Si2 O1 109.13(10) . . ?
O2 Si2 O1 106.20(10) . . ?
O8 Si2 C21 109.59(13) . . ?
O2 Si2 C21 111.09(13) . . ?
O1 Si2 C21 111.94(13) . . ?
O9 Si3 O2 108.83(11) . . ?
O9 Si3 O3 108.54(10) . . ?
O2 Si3 O3 106.42(11) . . ?
O9 Si3 C31 109.76(13) . . ?
O2 Si3 C31 112.34(13) . . ?
O3 Si3 C31 110.83(12) . . ?
O7 Si4 O6 108.53(11) . . ?
O7 Si4 O4 108.99(11) . . ?
O6 Si4 O4 106.85(10) . . ?
O7 Si4 C41 109.87(12) . . ?
O6 Si4 C41 110.60(12) . . ?
O4 Si4 C41 111.90(12) . . ?
O8 Si5 O5 108.94(11) . . ?
O8 Si5 O4 108.38(10) . . ?
O5 Si5 O4 106.30(10) . . ?
O8 Si5 C51 110.51(13) . . ?
O5 Si5 C51 110.68(13) . . ?
O4 Si5 C51 111.89(12) . . ?
O9 Si6 O5 109.34(11) . . ?
O9 Si6 O6 109.09(10) . . ?
O5 Si6 O6 106.17(10) . . ?
O9 Si6 C61 109.59(13) . . ?
O5 Si6 C61 113.15(13) . . ?
O6 Si6 C61 109.38(13) . . ?
Si1 O1 Si2 129.73(13) . . ?
Si3 O2 Si2 130.18(12) . . ?
Si3 O3 Si1 131.12(13) . . ?
Si4 O4 Si5 129.69(13) . . ?
Si6 O5 Si5 130.04(12) . . ?
Si4 O6 Si6 131.18(13) . . ?
Si4 O7 Si1 137.10(12) . . ?
Si5 O8 Si2 141.08(13) . . ?
Si6 O9 Si3 137.58(13) . . ?
C12 C11 C14 109.3(3) . . ?
C12 C11 C13 109.7(3) . . ?
C14 C11 C13 109.2(3) . . ?
C12 C11 Si1 109.5(2) . . ?
C14 C11 Si1 109.2(2) . . ?
C13 C11 Si1 109.9(2) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C24 C21 C23 109.3(3) . . ?
C24 C21 C22 109.0(3) . . ?
C23 C21 C22 109.4(3) . . ?
C24 C21 Si2 110.1(2) . . ?
C23 C21 Si2 109.7(2) . . ?
C22 C21 Si2 109.3(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C34 C31 C33 109.6(3) . . ?
C34 C31 C32 109.5(3) . . ?
C33 C31 C32 109.6(3) . . ?
C34 C31 Si3 110.1(2) . . ?
C33 C31 Si3 108.6(2) . . ?
C32 C31 Si3 109.5(2) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C43 C41 C44 109.5(3) . . ?
C43 C41 C42 109.9(3) . . ?
C44 C41 C42 109.6(3) . . ?
C43 C41 Si4 110.2(2) . . ?
C44 C41 Si4 108.5(2) . . ?
C42 C41 Si4 109.2(2) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C53 C51 C54 110.1(3) . . ?
C53 C51 C52 109.4(3) . . ?
C54 C51 C52 109.4(3) . . ?
C53 C51 Si5 109.7(2) . . ?
C54 C51 Si5 109.7(2) . . ?
C52 C51 Si5 108.5(2) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C64 C61 C62 109.5(3) . . ?
C64 C61 C63 109.7(3) . . ?
C62 C61 C63 109.3(3) . . ?
C64 C61 Si6 110.1(2) . . ?
C62 C61 Si6 111.0(2) . . ?
C63 C61 Si6 107.1(2) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?

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
O7 Si1 O1 Si2 91.71(17) . . . . ?
O3 Si1 O1 Si2 -26.20(19) . . . . ?
C11 Si1 O1 Si2 -147.31(17) . . . . ?
O8 Si2 O1 Si1 -88.43(18) . . . . ?
O2 Si2 O1 Si1 28.69(19) . . . . ?
C21 Si2 O1 Si1 150.09(17) . . . . ?
O9 Si3 O2 Si2 -91.03(17) . . . . ?
O3 Si3 O2 Si2 25.75(19) . . . . ?
C31 Si3 O2 Si2 147.21(17) . . . . ?
O8 Si2 O2 Si3 88.86(17) . . . . ?
O1 Si2 O2 Si3 -28.49(19) . . . . ?
C21 Si2 O2 Si3 -150.42(17) . . . . ?
O9 Si3 O3 Si1 94.59(18) . . . . ?
O2 Si3 O3 Si1 -22.4(2) . . . . ?
C31 Si3 O3 Si1 -144.81(17) . . . . ?
O7 Si1 O3 Si3 -94.68(17) . . . . ?
O1 Si1 O3 Si3 22.7(2) . . . . ?
C11 Si1 O3 Si3 144.68(17) . . . . ?
O7 Si4 O4 Si5 -92.37(17) . . . . ?
O6 Si4 O4 Si5 24.72(19) . . . . ?
C41 Si4 O4 Si5 145.91(17) . . . . ?
O8 Si5 O4 Si4 89.24(18) . . . . ?
O5 Si5 O4 Si4 -27.72(19) . . . . ?
C51 Si5 O4 Si4 -148.66(17) . . . . ?
O9 Si6 O5 Si5 90.87(17) . . . . ?
O6 Si6 O5 Si5 -26.70(19) . . . . ?
C61 Si6 O5 Si5 -146.68(17) . . . . ?
O8 Si5 O5 Si6 -87.54(17) . . . . ?
O4 Si5 O5 Si6 29.05(19) . . . . ?
C51 Si5 O5 Si6 150.76(17) . . . . ?
O7 Si4 O6 Si6 95.53(17) . . . . ?
O4 Si4 O6 Si6 -21.86(19) . . . . ?
C41 Si4 O6 Si6 -143.88(17) . . . . ?
O9 Si6 O6 Si4 -95.16(18) . . . . ?
O5 Si6 O6 Si4 22.6(2) . . . . ?
C61 Si6 O6 Si4 144.97(17) . . . . ?
O6 Si4 O7 Si1 -52.7(2) . . . . ?
O4 Si4 O7 Si1 63.4(2) . . . . ?
C41 Si4 O7 Si1 -173.70(18) . . . . ?
O3 Si1 O7 Si4 52.5(2) . . . . ?
O1 Si1 O7 Si4 -63.4(2) . . . . ?
C11 Si1 O7 Si4 173.90(19) . . . . ?
O5 Si5 O8 Si2 57.8(2) . . . . ?
O4 Si5 O8 Si2 -57.4(2) . . . . ?
C51 Si5 O8 Si2 179.7(2) . . . . ?
O2 Si2 O8 Si5 -58.3(2) . . . . ?
O1 Si2 O8 Si5 57.2(2) . . . . ?
C21 Si2 O8 Si5 -179.9(2) . . . . ?
O5 Si6 O9 Si3 -63.3(2) . . . . ?
O6 Si6 O9 Si3 52.4(2) . . . . ?
C61 Si6 O9 Si3 172.12(18) . . . . ?
O2 Si3 O9 Si6 62.8(2) . . . . ?
O3 Si3 O9 Si6 -52.7(2) . . . . ?
C31 Si3 O9 Si6 -173.92(18) . . . . ?
O7 Si1 C11 C12 179.0(2) . . . . ?
O3 Si1 C11 C12 -60.2(2) . . . . ?
O1 Si1 C11 C12 58.4(2) . . . . ?
O7 Si1 C11 C14 -61.3(2) . . . . ?
O3 Si1 C11 C14 59.5(2) . . . . ?
O1 Si1 C11 C14 178.1(2) . . . . ?
O7 Si1 C11 C13 58.5(2) . . . . ?
O3 Si1 C11 C13 179.3(2) . . . . ?
O1 Si1 C11 C13 -62.1(2) . . . . ?
O8 Si2 C21 C24 -177.7(2) . . . . ?
O2 Si2 C21 C24 62.1(3) . . . . ?
O1 Si2 C21 C24 -56.4(3) . . . . ?
O8 Si2 C21 C23 -57.3(3) . . . . ?
O2 Si2 C21 C23 -177.5(2) . . . . ?
O1 Si2 C21 C23 63.9(3) . . . . ?
O8 Si2 C21 C22 62.6(3) . . . . ?
O2 Si2 C21 C22 -57.6(3) . . . . ?
O1 Si2 C21 C22 -176.1(2) . . . . ?
O9 Si3 C31 C34 179.3(2) . . . . ?
O2 Si3 C31 C34 -59.5(2) . . . . ?
O3 Si3 C31 C34 59.4(2) . . . . ?
O9 Si3 C31 C33 59.3(2) . . . . ?
O2 Si3 C31 C33 -179.5(2) . . . . ?
O3 Si3 C31 C33 -60.6(2) . . . . ?
O9 Si3 C31 C32 -60.3(3) . . . . ?
O2 Si3 C31 C32 60.9(3) . . . . ?
O3 Si3 C31 C32 179.8(2) . . . . ?
O7 Si4 C41 C43 -176.0(2) . . . . ?
O6 Si4 C41 C43 64.2(2) . . . . ?
O4 Si4 C41 C43 -54.8(2) . . . . ?
O7 Si4 C41 C44 64.2(2) . . . . ?
O6 Si4 C41 C44 -55.6(2) . . . . ?
O4 Si4 C41 C44 -174.6(2) . . . . ?
O7 Si4 C41 C42 -55.2(2) . . . . ?
O6 Si4 C41 C42 -175.0(2) . . . . ?
O4 Si4 C41 C42 66.0(2) . . . . ?
O8 Si5 C51 C53 174.9(2) . . . . ?
O5 Si5 C51 C53 -64.3(2) . . . . ?
O4 Si5 C51 C53 54.0(2) . . . . ?
O8 Si5 C51 C54 53.8(2) . . . . ?
O5 Si5 C51 C54 174.6(2) . . . . ?
O4 Si5 C51 C54 -67.0(2) . . . . ?
O8 Si5 C51 C52 -65.7(3) . . . . ?
O5 Si5 C51 C52 55.1(3) . . . . ?
O4 Si5 C51 C52 173.5(2) . . . . ?
O9 Si6 C61 C64 176.9(2) . . . . ?
O5 Si6 C61 C64 54.6(3) . . . . ?
O6 Si6 C61 C64 -63.6(2) . . . . ?
O9 Si6 C61 C62 55.4(3) . . . . ?
O5 Si6 C61 C62 -66.9(3) . . . . ?
O6 Si6 C61 C62 175.0(2) . . . . ?
O9 Si6 C61 C63 -63.8(2) . . . . ?
O5 Si6 C61 C63 173.9(2) . . . . ?
O6 Si6 C61 C63 55.7(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.066

#==============================================================================

data_rp001_hy
_database_code_depnum_ccdc_archive 'CCDC 682321'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Hepta-tert.butyl-tricyclo[7.3.3.1(5,11)]heptasiloxane-ende-endo-3,7,14-triol
;
_chemical_name_common            
;Hepta-tert.butyl-tricyclo(7.3.3.1(5,11))heptasiloxane-ende-
endo-3,7,14-triol
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H66 O12 Si7'
_chemical_formula_sum            'C28 H66 O12 Si7'
_chemical_formula_weight         791.44

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           trigonal
_symmetry_space_group_name_H-M   R-3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   13.2424(15)
_cell_length_b                   13.2424(15)
_cell_length_c                   90.514(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     13746(2)
_cell_formula_units_Z            12
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    303
_cell_measurement_theta_min      1
_cell_measurement_theta_max      25

_exptl_crystal_description       blocks
_exptl_crystal_colour            yellowish
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5136
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
dx = 55 mm, 120 sec./deg.,1 deg., 5 sets, 630 frames,
scaling unsing SADABS (T-ratio = 0.6977)
;

_diffrn_ambient_temperature      123(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  'Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 1 deg.'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25425
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -107
_diffrn_reflns_limit_l_max       107
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         25.02
_reflns_number_total             2697
_reflns_number_gt                1812
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Collect
_computing_cell_refinement       DIRAX
_computing_data_reduction        EVALCCD
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.0237P)^2^+129.5700P] 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         2697
_refine_ls_number_parameters     145
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0604
_refine_ls_wR_factor_ref         0.1380
_refine_ls_wR_factor_gt          0.1172
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_restrained_S_all      1.167
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 1.0000 1.0000 0.06246(2) 0.0230(5) Uani 1 3 d S . .
Si2 Si 0.84674(10) 0.78225(10) 0.042632(12) 0.0219(3) Uani 1 1 d . . .
Si3 Si 0.76161(9) 0.92836(10) 0.024338(11) 0.0203(3) Uani 1 1 d . . .
O1 O 0.9048(2) 0.8716(2) 0.05637(3) 0.0293(7) Uani 1 1 d . . .
O2 O 0.9504(2) 0.7812(2) 0.03321(3) 0.0273(7) Uani 1 1 d . . .
O3 O 0.7767(2) 0.8268(2) 0.03222(3) 0.0257(7) Uani 1 1 d . . .
O4 O 0.8159(3) 0.9498(3) 0.00777(3) 0.0349(8) Uani 1 1 d D . .
H4 H 0.824(5) 0.895(3) 0.0046(5) 0.052 Uiso 1 1 d D . .
C11 C 1.0000 1.0000 0.08295(8) 0.051(3) Uani 1 3 d S . .
C12 C 0.8807(6) 0.9757(7) 0.08856(5) 0.091(3) Uani 1 1 d . . .
H12A H 0.8203 0.8986 0.0851 0.136 Uiso 1 1 calc R . .
H12B H 0.8644 1.0353 0.0847 0.136 Uiso 1 1 calc R . .
H12C H 0.8812 0.9775 0.0994 0.136 Uiso 1 1 calc R . .
C21 C 0.7447(4) 0.6322(4) 0.04965(5) 0.0337(11) Uani 1 1 d . . .
C22 C 0.6912(5) 0.5488(4) 0.03655(6) 0.0515(14) Uani 1 1 d . . .
H22A H 0.7534 0.5485 0.0307 0.077 Uiso 1 1 calc R . .
H22B H 0.6478 0.5746 0.0303 0.077 Uiso 1 1 calc R . .
H22C H 0.6382 0.4699 0.0402 0.077 Uiso 1 1 calc R . .
C23 C 0.8114(5) 0.5900(4) 0.05942(6) 0.0561(15) Uani 1 1 d . . .
H23A H 0.8730 0.5885 0.0536 0.084 Uiso 1 1 calc R . .
H23B H 0.7574 0.5114 0.0631 0.084 Uiso 1 1 calc R . .
H23C H 0.8463 0.6432 0.0678 0.084 Uiso 1 1 calc R . .
C24 C 0.6474(5) 0.6331(5) 0.05882(6) 0.0560(16) Uani 1 1 d . . .
H24A H 0.6818 0.6860 0.0672 0.084 Uiso 1 1 calc R . .
H24B H 0.5939 0.5542 0.0624 0.084 Uiso 1 1 calc R . .
H24C H 0.6045 0.6596 0.0526 0.084 Uiso 1 1 calc R . .
C31 C 0.6040(4) 0.8822(4) 0.02301(5) 0.0280(10) Uani 1 1 d . . .
C32 C 0.5469(4) 0.8599(5) 0.03825(5) 0.0475(13) Uani 1 1 d . . .
H32A H 0.5871 0.9310 0.0442 0.071 Uiso 1 1 calc R . .
H32B H 0.5523 0.7968 0.0432 0.071 Uiso 1 1 calc R . .
H32C H 0.4647 0.8377 0.0371 0.071 Uiso 1 1 calc R . .
C33 C 0.5420(4) 0.7703(4) 0.01360(5) 0.0487(13) Uani 1 1 d . . .
H33A H 0.5493 0.7080 0.0184 0.073 Uiso 1 1 calc R . .
H33B H 0.5781 0.7854 0.0038 0.073 Uiso 1 1 calc R . .
H33C H 0.4594 0.7464 0.0126 0.073 Uiso 1 1 calc R . .
C34 C 0.5906(4) 0.9778(4) 0.01516(6) 0.0448(13) Uani 1 1 d . . .
H34A H 0.6304 1.0501 0.0209 0.067 Uiso 1 1 calc R . .
H34B H 0.5077 0.9531 0.0143 0.067 Uiso 1 1 calc R . .
H34C H 0.6253 0.9911 0.0053 0.067 Uiso 1 1 calc R . .

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
Si1 0.0290(7) 0.0290(7) 0.0110(9) 0.000 0.000 0.0145(3)
Si2 0.0204(6) 0.0202(6) 0.0249(6) 0.0066(5) 0.0041(5) 0.0099(5)
Si3 0.0207(6) 0.0195(6) 0.0207(6) 0.0015(5) 0.0025(5) 0.0101(5)
O1 0.0350(18) 0.0258(16) 0.0217(14) 0.0047(12) 0.0029(13) 0.0113(14)
O2 0.0222(16) 0.0240(16) 0.0366(16) 0.0056(13) 0.0067(13) 0.0123(14)
O3 0.0219(15) 0.0217(16) 0.0326(15) 0.0054(13) 0.0037(13) 0.0103(13)
O4 0.0435(19) 0.0359(19) 0.0289(16) 0.0020(14) 0.0112(15) 0.0226(17)
C11 0.069(4) 0.069(4) 0.017(4) 0.000 0.000 0.034(2)
C12 0.104(6) 0.144(7) 0.027(3) 0.012(4) 0.033(3) 0.064(5)
C21 0.032(3) 0.025(2) 0.043(3) 0.015(2) 0.011(2) 0.013(2)
C22 0.044(3) 0.022(3) 0.069(4) 0.006(3) 0.001(3) 0.002(2)
C23 0.057(4) 0.034(3) 0.071(4) 0.030(3) 0.004(3) 0.018(3)
C24 0.042(3) 0.044(3) 0.071(4) 0.026(3) 0.031(3) 0.013(3)
C31 0.024(2) 0.028(2) 0.033(2) 0.0013(19) -0.0034(19) 0.014(2)
C32 0.026(3) 0.061(4) 0.059(3) 0.016(3) 0.017(2) 0.024(3)
C33 0.032(3) 0.034(3) 0.074(3) -0.014(3) -0.016(3) 0.012(2)
C34 0.032(3) 0.037(3) 0.067(3) 0.006(3) -0.012(3) 0.018(2)

_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
Si1 O1 1.625(3) 2_765 ?
Si1 O1 1.625(3) . ?
Si1 O1 1.625(3) 3_675 ?
Si1 C11 1.855(8) . ?
Si2 O1 1.621(3) . ?
Si2 O2 1.623(3) . ?
Si2 O3 1.627(3) . ?
Si2 C21 1.869(4) . ?
Si3 O2 1.609(3) 3_675 ?
Si3 O3 1.620(3) . ?
Si3 O4 1.626(3) . ?
Si3 C31 1.863(4) . ?
O2 Si3 1.609(3) 2_765 ?
O4 H4 0.833(19) . ?
C11 C12 1.532(7) 3_675 ?
C11 C12 1.532(7) 2_765 ?
C11 C12 1.532(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 C22 1.532(6) . ?
C21 C23 1.538(6) . ?
C21 C24 1.538(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C31 C32 1.529(6) . ?
C31 C34 1.537(6) . ?
C31 C33 1.542(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Si1 O1 109.11(11) 2_765 . ?
O1 Si1 O1 109.11(11) 2_765 3_675 ?
O1 Si1 O1 109.11(11) . 3_675 ?
O1 Si1 C11 109.83(11) 2_765 . ?
O1 Si1 C11 109.83(11) . . ?
O1 Si1 C11 109.83(11) 3_675 . ?
O1 Si2 O2 108.38(16) . . ?
O1 Si2 O3 109.12(15) . . ?
O2 Si2 O3 109.73(14) . . ?
O1 Si2 C21 110.01(18) . . ?
O2 Si2 C21 109.52(18) . . ?
O3 Si2 C21 110.05(18) . . ?
O2 Si3 O3 111.31(15) 3_675 . ?
O2 Si3 O4 107.74(16) 3_675 . ?
O3 Si3 O4 108.93(16) . . ?
O2 Si3 C31 110.16(17) 3_675 . ?
O3 Si3 C31 109.80(17) . . ?
O4 Si3 C31 108.84(18) . . ?
Si2 O1 Si1 149.39(19) . . ?
Si3 O2 Si2 157.8(2) 2_765 . ?
Si3 O3 Si2 152.34(19) . . ?
Si3 O4 H4 113(3) . . ?
C12 C11 C12 109.6(3) 3_675 2_765 ?
C12 C11 C12 109.6(3) 3_675 . ?
C12 C11 C12 109.6(3) 2_765 . ?
C12 C11 Si1 109.3(3) 3_675 . ?
C12 C11 Si1 109.3(3) 2_765 . ?
C12 C11 Si1 109.3(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C22 C21 C23 109.0(4) . . ?
C22 C21 C24 109.6(4) . . ?
C23 C21 C24 109.2(4) . . ?
C22 C21 Si2 109.3(3) . . ?
C23 C21 Si2 109.9(3) . . ?
C24 C21 Si2 109.8(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C32 C31 C34 109.1(4) . . ?
C32 C31 C33 109.8(4) . . ?
C34 C31 C33 108.1(4) . . ?
C32 C31 Si3 111.7(3) . . ?
C34 C31 Si3 109.3(3) . . ?
C33 C31 Si3 108.7(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

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
O2 Si2 O1 Si1 51.4(4) . . . . ?
O3 Si2 O1 Si1 -68.0(4) . . . . ?
C21 Si2 O1 Si1 171.2(4) . . . . ?
O1 Si1 O1 Si2 -52.2(4) 2_765 . . . ?
O1 Si1 O1 Si2 66.9(4) 3_675 . . . ?
C11 Si1 O1 Si2 -172.7(3) . . . . ?
O1 Si2 O2 Si3 -50.3(5) . . . 2_765 ?
O3 Si2 O2 Si3 68.7(5) . . . 2_765 ?
C21 Si2 O2 Si3 -170.4(5) . . . 2_765 ?
O2 Si3 O3 Si2 -25.0(4) 3_675 . . . ?
O4 Si3 O3 Si2 93.7(4) . . . . ?
C31 Si3 O3 Si2 -147.2(4) . . . . ?
O1 Si2 O3 Si3 37.5(4) . . . . ?
O2 Si2 O3 Si3 -81.1(4) . . . . ?
C21 Si2 O3 Si3 158.3(4) . . . . ?
O1 Si1 C11 C12 56.7(3) 2_765 . . 3_675 ?
O1 Si1 C11 C12 176.7(3) . . . 3_675 ?
O1 Si1 C11 C12 -63.3(3) 3_675 . . 3_675 ?
O1 Si1 C11 C12 -63.3(3) 2_765 . . 2_765 ?
O1 Si1 C11 C12 56.7(3) . . . 2_765 ?
O1 Si1 C11 C12 176.7(3) 3_675 . . 2_765 ?
O1 Si1 C11 C12 176.7(3) 2_765 . . . ?
O1 Si1 C11 C12 -63.3(3) . . . . ?
O1 Si1 C11 C12 56.7(3) 3_675 . . . ?
O1 Si2 C21 C22 -179.7(3) . . . . ?
O2 Si2 C21 C22 -60.7(4) . . . . ?
O3 Si2 C21 C22 60.0(4) . . . . ?
O1 Si2 C21 C23 -60.0(4) . . . . ?
O2 Si2 C21 C23 59.0(4) . . . . ?
O3 Si2 C21 C23 179.7(3) . . . . ?
O1 Si2 C21 C24 60.0(4) . . . . ?
O2 Si2 C21 C24 179.0(3) . . . . ?
O3 Si2 C21 C24 -60.3(4) . . . . ?
O2 Si3 C31 C32 -62.3(4) 3_675 . . . ?
O3 Si3 C31 C32 60.6(4) . . . . ?
O4 Si3 C31 C32 179.8(3) . . . . ?
O2 Si3 C31 C34 58.5(3) 3_675 . . . ?
O3 Si3 C31 C34 -178.6(3) . . . . ?
O4 Si3 C31 C34 -59.4(3) . . . . ?
O2 Si3 C31 C33 176.4(3) 3_675 . . . ?
O3 Si3 C31 C33 -60.7(3) . . . . ?
O4 Si3 C31 C33 58.4(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O4 0.833(19) 1.80(2) 2.596(4) 158(5) 21_655

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.083