# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005


data_global
_journal_name_full               Chem.Commun.
#==============================================================================
_journal_coden_Cambridge         0182

_audit_creation_date             07-23-2005

# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Louis Ricard'
_publ_contact_author_address     
;Laboratoire DCPH
Ecole Polytechnique
Route de Saclay
F91128 Palaiseau
France
;
_publ_contact_author_email       louis.ricard@polytechnique.fr
_publ_contact_author_phone       330169334572
_publ_contact_author_fax         330169333990

#==============================================================================
# 2. PROCESSING SUMMARY (IUCr Office Use Only)

#==============================================================================
# 3. TITLE AND AUTHOR LIST

_publ_section_title              
;
Reversal of Facial Selectivity in Complex Diels-Alder Reaction.
;
# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.

loop_
_publ_author_name
_publ_author_address
J.A.Funel
;
Laboratoire de Synthese Organique,
CNRS UMR 7652
DCSO Ecole Polytechnique,
F-91128 Palaiseau Cedex
France
;
L.Ricard
;
Laboratoire Heteroelements et Coordination,
CNRS UMR 7653,
DCPH Ecole Polytechnique,
F-91128 Palaiseau Cedex
France
;
J.Prunet
;
Laboratoire de Synthese Organique,
CNRS UMR 7652
DCSO Ecole Polytechnique,
F-91128 Palaiseau Cedex
France
;

#==============================================================================
# 4. TEXT

_publ_section_abstract           
; ?
;

_publ_section_comment            
;
;
_publ_section_exptl_prep         
;All structures were solved using SIR97 (Altomare et al.) and refined with
SHELXL97 (Sheldrick). Figures were drawn with Platon (Spek, 1990).
;

_publ_section_references         
;Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A.
(1993) J. Appl. Cryst. 26, 343-350.

Sheldrick, G.M. SHELXL97. Program for crystal structure
refinement. University of G\\"ottingen, Germany, 1997.

Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201.

Spek, A.L. (1990). Acta Cryst. A46, C-34.
;

_publ_section_figure_captions    
; ?
;

_publ_section_acknowledgements   
; ?
;

#==============================================================================
# If more than one structure is reported, sections 5-10 should be filled in
# per structure. For each data set, replace the ? in the data_? line below
# by a unique identifier.

#=============================================================================
data_jaf389
_database_code_depnum_ccdc_archive 'CCDC 247812'
#compound 9a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H21 Br O4'
_chemical_formula_weight         381.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P21/c '

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

_cell_length_a                   9.1750(10)
_cell_length_b                   15.3160(10)
_cell_length_c                   11.4560(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.2600(10)
_cell_angle_gamma                90.00
_cell_volume                     1573.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    251
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      20.0

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
_exptl_absorpt_coefficient_mu    2.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5952
_exptl_absorpt_correction_T_max  0.8171
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7595
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.46
_diffrn_reflns_theta_max         30.01
_reflns_number_total             4570
_reflns_number_gt                3526
_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.

The coordinates of hydrogen atoms H1 and H2 were located in a difference
Fourier map and refined with fixed U's.
;

_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^)+(0.0326P)^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    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0017(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4570
_refine_ls_number_parameters     221
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0769
_refine_ls_wR_factor_gt          0.0719
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
Br1 Br 0.613806(19) 0.469475(12) 0.386768(16) 0.02712(8) Uani 1 1 d . A .
O1 O 1.24626(14) 0.33428(11) 0.25109(12) 0.0357(4) Uani 1 1 d . . .
H1 H 1.329(2) 0.3487(16) 0.244(2) 0.054 Uiso 1 1 d . . .
O2 O 1.02772(13) 0.24425(9) 0.57200(12) 0.0307(3) Uani 1 1 d . . .
H2 H 1.088(2) 0.2191(15) 0.625(2) 0.046 Uiso 1 1 d . . .
O3 O 0.75094(15) 0.46153(9) 0.10916(12) 0.0336(3) Uani 1 1 d . . .
O4 O 0.50243(12) 0.35492(8) 0.16460(11) 0.0241(3) Uani 1 1 d . . .
C1 C 1.21299(18) 0.36028(13) 0.36193(16) 0.0257(4) Uani 1 1 d . . .
H1A H 1.2872 0.4046 0.4015 0.031 Uiso 1 1 calc R . .
C2 C 1.20782(18) 0.28415(13) 0.44692(17) 0.0268(4) Uani 1 1 d . . .
H2A H 1.3080 0.2726 0.4969 0.032 Uiso 1 1 calc R . .
H2B H 1.1712 0.2305 0.4019 0.032 Uiso 1 1 calc R . .
C3 C 1.09962(19) 0.31346(12) 0.52421(16) 0.0245(4) Uani 1 1 d . . .
H3 H 1.1558 0.3495 0.5918 0.029 Uiso 1 1 calc R . .
C4 C 0.98355(17) 0.37261(12) 0.44270(15) 0.0191(3) Uani 1 1 d . . .
H4 H 0.9666 0.4262 0.4879 0.023 Uiso 1 1 calc R . .
C5 C 1.05760(18) 0.39770(11) 0.34262(15) 0.0206(4) Uani 1 1 d . A .
C6 C 0.98254(18) 0.43408(12) 0.24328(16) 0.0232(4) Uani 1 1 d . . .
H6 H 1.0304 0.4433 0.1785 0.028 Uiso 1 1 calc R A .
C7 C 0.82261(18) 0.46102(12) 0.23134(16) 0.0224(4) Uani 1 1 d . A .
H7 H 0.8200 0.5215 0.2638 0.027 Uiso 1 1 calc R . .
C8 C 0.73455(17) 0.39826(11) 0.30107(14) 0.0184(3) Uani 1 1 d . . .
C9 C 0.83110(16) 0.33088(11) 0.38587(14) 0.0178(3) Uani 1 1 d . A .
H9 H 0.7783 0.3150 0.4508 0.021 Uiso 1 1 calc R . .
C10 C 0.83757(17) 0.24954(11) 0.30668(15) 0.0187(3) Uani 1 1 d . . .
H10 H 0.9393 0.2449 0.2887 0.022 Uiso 1 1 calc R A .
C11 C 0.72024(16) 0.26225(11) 0.18783(15) 0.0187(3) Uani 1 1 d . A .
H11 H 0.7703 0.2716 0.1194 0.022 Uiso 1 1 calc R . .
C12 C 0.63263(17) 0.34101(11) 0.20795(14) 0.0185(3) Uani 1 1 d . A .
C13 C 0.63052(18) 0.17514(12) 0.17279(15) 0.0219(4) Uani 1 1 d . . .
H13 H 0.5749 0.1610 0.0901 0.026 Uiso 1 1 calc R A .
C14 C 0.75482(19) 0.11098(12) 0.22917(17) 0.0277(4) Uani 1 1 d . A .
H14A H 0.8393 0.1106 0.1879 0.033 Uiso 1 1 calc R . .
H14B H 0.7177 0.0509 0.2357 0.033 Uiso 1 1 calc R . .
C15 C 0.79137(18) 0.15915(12) 0.35026(16) 0.0245(4) Uani 1 1 d . A .
H15 H 0.8668 0.1303 0.4146 0.029 Uiso 1 1 calc R . .
C16 C 0.63509(18) 0.16698(12) 0.37382(16) 0.0251(4) Uani 1 1 d . . .
H16 H 0.6097 0.1662 0.4500 0.030 Uiso 1 1 calc R A .
C17 C 0.54016(19) 0.17518(12) 0.26927(16) 0.0232(4) Uani 1 1 d . A .
H17 H 0.4348 0.1802 0.2572 0.028 Uiso 1 1 calc R . .
C18 C 0.7573(5) 0.5426(3) 0.0536(4) 0.0410(8) Uani 0.532(3) 1 d P A 1
H18A H 0.6881 0.5426 -0.0244 0.062 Uiso 0.532(3) 1 calc PR A 1
H18B H 0.8590 0.5529 0.0427 0.062 Uiso 0.532(3) 1 calc PR A 1
H18C H 0.7292 0.5888 0.1037 0.062 Uiso 0.532(3) 1 calc PR A 1
C19 C 0.6527(5) 0.5243(3) 0.0656(5) 0.0410(8) Uani 0.468(3) 1 d P A 2
H19A H 0.5693 0.5225 0.1067 0.062 Uiso 0.468(3) 1 calc PR A 2
H19B H 0.6152 0.5149 -0.0201 0.062 Uiso 0.468(3) 1 calc PR A 2
H19C H 0.7018 0.5814 0.0784 0.062 Uiso 0.468(3) 1 calc PR A 2

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
Br1 0.03157(12) 0.02528(12) 0.02672(11) -0.00111(7) 0.01117(8) 0.00906(7)
O1 0.0204(7) 0.0600(11) 0.0291(8) -0.0129(7) 0.0108(5) -0.0086(7)
O2 0.0231(7) 0.0349(8) 0.0323(8) 0.0145(6) 0.0020(5) -0.0006(6)
O3 0.0415(8) 0.0300(8) 0.0248(7) 0.0107(6) -0.0032(6) -0.0038(6)
O4 0.0174(6) 0.0288(7) 0.0252(7) 0.0042(5) 0.0025(5) 0.0021(5)
C1 0.0195(8) 0.0336(11) 0.0245(10) -0.0062(8) 0.0057(7) -0.0066(8)
C2 0.0151(8) 0.0306(11) 0.0332(10) -0.0016(8) 0.0019(7) 0.0004(7)
C3 0.0214(8) 0.0282(10) 0.0226(9) 0.0008(8) 0.0019(6) -0.0034(8)
C4 0.0191(8) 0.0188(9) 0.0194(8) -0.0026(7) 0.0043(6) -0.0024(7)
C5 0.0192(8) 0.0189(9) 0.0245(9) -0.0038(7) 0.0066(6) -0.0071(7)
C6 0.0246(9) 0.0233(10) 0.0236(9) -0.0015(7) 0.0095(7) -0.0054(7)
C7 0.0264(9) 0.0172(9) 0.0235(9) 0.0007(7) 0.0048(7) -0.0015(7)
C8 0.0196(8) 0.0166(9) 0.0202(8) -0.0012(7) 0.0071(6) 0.0034(7)
C9 0.0180(8) 0.0179(9) 0.0177(8) 0.0017(6) 0.0045(6) -0.0004(6)
C10 0.0152(8) 0.0183(9) 0.0217(9) -0.0010(7) 0.0021(6) 0.0017(6)
C11 0.0173(8) 0.0205(9) 0.0189(8) -0.0017(7) 0.0053(6) 0.0001(7)
C12 0.0201(8) 0.0200(9) 0.0163(8) 0.0048(7) 0.0058(6) -0.0009(7)
C13 0.0221(9) 0.0224(10) 0.0204(9) -0.0039(7) 0.0025(6) -0.0017(7)
C14 0.0273(9) 0.0188(10) 0.0356(11) -0.0047(8) 0.0036(7) 0.0000(7)
C15 0.0256(9) 0.0189(9) 0.0260(10) -0.0002(7) -0.0013(7) -0.0017(7)
C16 0.0306(10) 0.0205(10) 0.0242(10) 0.0026(7) 0.0060(7) -0.0063(7)
C17 0.0213(8) 0.0193(9) 0.0289(10) -0.0017(7) 0.0053(7) -0.0058(7)
C18 0.0447(19) 0.0335(18) 0.0444(19) 0.0168(14) 0.0082(15) 0.0010(15)
C19 0.0447(19) 0.0335(18) 0.0444(19) 0.0168(14) 0.0082(15) 0.0010(15)

_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
Br1 C8 1.9602(16) . ?
O1 C1 1.424(2) . ?
O1 H1 0.81(2) . ?
O2 C3 1.418(2) . ?
O2 H2 0.83(2) . ?
O3 C19 1.339(4) . ?
O3 C18 1.402(4) . ?
O3 C7 1.414(2) . ?
O4 C12 1.2112(18) . ?
C1 C5 1.509(2) . ?
C1 C2 1.526(3) . ?
C1 H1A 1.0000 . ?
C2 C3 1.531(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.551(2) . ?
C3 H3 1.0000 . ?
C4 C5 1.501(2) . ?
C4 C9 1.550(2) . ?
C4 H4 1.0000 . ?
C5 C6 1.322(2) . ?
C6 C7 1.502(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.578(2) . ?
C7 H7 1.0000 . ?
C8 C12 1.535(2) . ?
C8 C9 1.558(2) . ?
C9 C10 1.550(2) . ?
C9 H9 1.0000 . ?
C10 C11 1.558(2) . ?
C10 C15 1.561(2) . ?
C10 H10 1.0000 . ?
C11 C12 1.494(2) . ?
C11 C13 1.558(2) . ?
C11 H11 1.0000 . ?
C13 C17 1.516(2) . ?
C13 C14 1.540(2) . ?
C13 H13 1.0000 . ?
C14 C15 1.544(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.519(2) . ?
C15 H15 1.0000 . ?
C16 C17 1.329(2) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 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
C1 O1 H1 113.5(17) . . ?
C3 O2 H2 109.6(16) . . ?
C19 O3 C18 44.3(3) . . ?
C19 O3 C7 120.5(3) . . ?
C18 O3 C7 113.5(2) . . ?
O1 C1 C5 110.50(14) . . ?
O1 C1 C2 113.37(16) . . ?
C5 C1 C2 103.14(13) . . ?
O1 C1 H1A 109.9 . . ?
C5 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
C1 C2 C3 104.88(15) . . ?
C1 C2 H2A 110.8 . . ?
C3 C2 H2A 110.8 . . ?
C1 C2 H2B 110.8 . . ?
C3 C2 H2B 110.8 . . ?
H2A C2 H2B 108.8 . . ?
O2 C3 C2 114.58(15) . . ?
O2 C3 C4 110.66(13) . . ?
C2 C3 C4 105.65(14) . . ?
O2 C3 H3 108.6 . . ?
C2 C3 H3 108.6 . . ?
C4 C3 H3 108.6 . . ?
C5 C4 C9 107.41(13) . . ?
C5 C4 C3 104.19(13) . . ?
C9 C4 C3 117.08(14) . . ?
C5 C4 H4 109.3 . . ?
C9 C4 H4 109.3 . . ?
C3 C4 H4 109.3 . . ?
C6 C5 C4 121.86(15) . . ?
C6 C5 C1 126.14(16) . . ?
C4 C5 C1 110.95(14) . . ?
C5 C6 C7 120.96(16) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
O3 C7 C6 109.35(15) . . ?
O3 C7 C8 108.90(13) . . ?
C6 C7 C8 112.45(14) . . ?
O3 C7 H7 108.7 . . ?
C6 C7 H7 108.7 . . ?
C8 C7 H7 108.7 . . ?
C12 C8 C9 103.69(13) . . ?
C12 C8 C7 107.34(13) . . ?
C9 C8 C7 115.77(13) . . ?
C12 C8 Br1 109.88(10) . . ?
C9 C8 Br1 111.30(11) . . ?
C7 C8 Br1 108.62(11) . . ?
C10 C9 C4 115.72(13) . . ?
C10 C9 C8 104.76(12) . . ?
C4 C9 C8 109.37(13) . . ?
C10 C9 H9 108.9 . . ?
C4 C9 H9 108.9 . . ?
C8 C9 H9 108.9 . . ?
C9 C10 C11 107.81(12) . . ?
C9 C10 C15 118.63(14) . . ?
C11 C10 C15 101.90(12) . . ?
C9 C10 H10 109.3 . . ?
C11 C10 H10 109.3 . . ?
C15 C10 H10 109.3 . . ?
C12 C11 C13 114.80(13) . . ?
C12 C11 C10 105.10(13) . . ?
C13 C11 C10 103.91(13) . . ?
C12 C11 H11 110.9 . . ?
C13 C11 H11 110.9 . . ?
C10 C11 H11 110.9 . . ?
O4 C12 C11 126.49(15) . . ?
O4 C12 C8 125.91(16) . . ?
C11 C12 C8 107.46(13) . . ?
C17 C13 C14 99.52(14) . . ?
C17 C13 C11 106.08(14) . . ?
C14 C13 C11 99.97(13) . . ?
C17 C13 H13 116.3 . . ?
C14 C13 H13 116.3 . . ?
C11 C13 H13 116.3 . . ?
C13 C14 C15 94.14(14) . . ?
C13 C14 H14A 112.9 . . ?
C15 C14 H14A 112.9 . . ?
C13 C14 H14B 112.9 . . ?
C15 C14 H14B 112.9 . . ?
H14A C14 H14B 110.3 . . ?
C16 C15 C14 99.45(13) . . ?
C16 C15 C10 108.51(14) . . ?
C14 C15 C10 99.12(14) . . ?
C16 C15 H15 115.8 . . ?
C14 C15 H15 115.8 . . ?
C10 C15 H15 115.8 . . ?
C17 C16 C15 108.06(16) . . ?
C17 C16 H16 126.0 . . ?
C15 C16 H16 126.0 . . ?
C16 C17 C13 107.57(15) . . ?
C16 C17 H17 126.2 . . ?
C13 C17 H17 126.2 . . ?
O3 C18 H18A 109.5 . . ?
O3 C18 H18B 109.5 . . ?
O3 C18 H18C 109.5 . . ?
O3 C19 H19A 109.5 . . ?
O3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

_diffrn_measured_fraction_theta_max .996
_diffrn_reflns_theta_full        30.01
_diffrn_measured_fraction_theta_full .996
_refine_diff_density_max         .437
_refine_diff_density_min         -.455
_refine_diff_density_rms         .070
#END===
data_jaf527
_database_code_depnum_ccdc_archive 'CCDC 247814'
#compound 12

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H45 N O4 Si2'
_chemical_formula_weight         527.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1 '

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

_cell_length_a                   11.2940(10)
_cell_length_b                   16.4190(10)
_cell_length_c                   17.5230(10)
_cell_angle_alpha                101.6800(10)
_cell_angle_beta                 102.9000(10)
_cell_angle_gamma                89.8000(10)
_cell_volume                     3098.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(10)
_cell_measurement_reflns_used    251
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      20.0

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9686
_exptl_absorpt_correction_T_max  0.9942
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150.0(10)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15402
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0714
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         22.98
_reflns_number_total             8593
_reflns_number_gt                5458
_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^)+(0.0651P)^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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8593
_refine_ls_number_parameters     669
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1223
_refine_ls_wR_factor_gt          0.1056
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_restrained_S_all      0.948
_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
Si1 Si -0.29398(7) 0.66807(5) 0.32216(5) 0.0427(2) Uani 1 1 d . . .
Si2 Si -0.22681(6) 0.20626(5) 0.32792(5) 0.0371(2) Uani 1 1 d . . .
Si3 Si 0.27630(7) 0.42684(5) 0.33397(5) 0.0405(2) Uani 1 1 d . . .
Si4 Si 0.20263(7) -0.03613(5) 0.31777(5) 0.0422(2) Uani 1 1 d . . .
O1 O -0.34845(15) 0.57197(11) 0.30890(11) 0.0411(5) Uani 1 1 d . . .
O2 O -0.35559(19) 0.40014(16) -0.06129(13) 0.0702(7) Uani 1 1 d . . .
O3 O -0.11167(18) 0.31181(15) 0.14697(13) 0.0605(6) Uani 1 1 d . . .
O4 O -0.30893(15) 0.28279(12) 0.30167(12) 0.0438(5) Uani 1 1 d . . .
O5 O 0.18979(15) 0.34092(11) 0.30289(11) 0.0432(5) Uani 1 1 d . . .
O6 O 0.14670(15) 0.05333(11) 0.30295(11) 0.0390(5) Uani 1 1 d . . .
O7 O 0.14230(19) 0.07571(15) -0.06283(13) 0.0665(7) Uani 1 1 d . . .
O8 O 0.38408(18) 0.25214(13) 0.14624(13) 0.0580(6) Uani 1 1 d . . .
N1 N -0.21088(19) 0.35674(14) 0.03509(13) 0.0409(6) Uani 1 1 d . . .
N2 N 0.28605(19) 0.16028(14) 0.03340(13) 0.0396(6) Uani 1 1 d . . .
C1 C -0.3298(3) 0.3709(2) -0.00263(19) 0.0484(8) Uani 1 1 d . . .
C2 C -0.4160(2) 0.34361(19) 0.04372(18) 0.0461(8) Uani 1 1 d . . .
H2 H -0.4686 0.2953 0.0089 0.055 Uiso 1 1 calc R . .
C3 C -0.4974(2) 0.41548(18) 0.06724(18) 0.0452(8) Uani 1 1 d . . .
H3A H -0.5271 0.4419 0.0209 0.054 Uiso 1 1 calc R . .
H3B H -0.5689 0.3931 0.0815 0.054 Uiso 1 1 calc R . .
C4 C -0.4295(2) 0.47959(18) 0.13670(17) 0.0408(7) Uani 1 1 d . . .
H4 H -0.4352 0.5374 0.1371 0.049 Uiso 1 1 calc R . .
C5 C -0.3610(2) 0.45235(17) 0.19764(16) 0.0362(7) Uani 1 1 d . . .
C6 C -0.2904(2) 0.49919(16) 0.27815(17) 0.0381(7) Uani 1 1 d . . .
H6 H -0.2073 0.5153 0.2736 0.046 Uiso 1 1 calc R . .
C7 C -0.2801(2) 0.43453(17) 0.33034(17) 0.0416(7) Uani 1 1 d . . .
H7A H -0.3529 0.4331 0.3527 0.050 Uiso 1 1 calc R . .
H7B H -0.2071 0.4468 0.3749 0.050 Uiso 1 1 calc R . .
C8 C -0.2698(2) 0.35235(17) 0.27391(16) 0.0381(7) Uani 1 1 d . . .
H8 H -0.1845 0.3459 0.2671 0.046 Uiso 1 1 calc R . .
C9 C -0.3551(2) 0.36089(16) 0.19523(16) 0.0351(7) Uani 1 1 d . . .
H9 H -0.4377 0.3416 0.1978 0.042 Uiso 1 1 calc R . .
C10 C -0.3334(2) 0.31419(18) 0.11481(17) 0.0427(7) Uani 1 1 d . . .
H10 H -0.3511 0.2534 0.1095 0.051 Uiso 1 1 calc R . .
C11 C -0.2057(3) 0.32631(18) 0.10471(18) 0.0440(7) Uani 1 1 d . . .
C12 C -0.1047(3) 0.36915(18) 0.00497(18) 0.0434(7) Uani 1 1 d . . .
C13 C -0.0037(3) 0.41284(19) 0.05532(19) 0.0468(8) Uani 1 1 d . . .
H13 H -0.0044 0.4368 0.1093 0.056 Uiso 1 1 calc R . .
C14 C 0.0995(3) 0.4215(2) 0.0262(2) 0.0539(9) Uani 1 1 d . . .
H14 H 0.1697 0.4514 0.0605 0.065 Uiso 1 1 calc R . .
C15 C 0.1000(3) 0.3870(2) -0.0517(2) 0.0645(10) Uani 1 1 d . . .
H15 H 0.1709 0.3927 -0.0711 0.077 Uiso 1 1 calc R . .
C16 C -0.0012(3) 0.3443(2) -0.1017(2) 0.0645(10) Uani 1 1 d . . .
H16 H 0.0000 0.3207 -0.1557 0.077 Uiso 1 1 calc R . .
C17 C -0.1052(3) 0.3350(2) -0.07415(19) 0.0556(9) Uani 1 1 d . . .
H17 H -0.1757 0.3058 -0.1089 0.067 Uiso 1 1 calc R . .
C18 C -0.1678(3) 0.6919(2) 0.4125(2) 0.0662(10) Uani 1 1 d . . .
H18A H -0.1968 0.6833 0.4591 0.099 Uiso 1 1 calc R . .
H18B H -0.1386 0.7499 0.4211 0.099 Uiso 1 1 calc R . .
H18C H -0.1011 0.6549 0.4049 0.099 Uiso 1 1 calc R . .
C19 C -0.2383(3) 0.6805(2) 0.2324(2) 0.0680(10) Uani 1 1 d . . .
H19A H -0.1754 0.6405 0.2241 0.102 Uiso 1 1 calc R . .
H19B H -0.2040 0.7372 0.2408 0.102 Uiso 1 1 calc R . .
H19C H -0.3061 0.6702 0.1853 0.102 Uiso 1 1 calc R . .
C20 C -0.4248(3) 0.73483(18) 0.33480(19) 0.0501(8) Uani 1 1 d . . .
C21 C -0.5319(3) 0.7089(2) 0.2618(2) 0.0779(11) Uani 1 1 d . . .
H21A H -0.6011 0.7431 0.2694 0.117 Uiso 1 1 calc R . .
H21B H -0.5552 0.6501 0.2559 0.117 Uiso 1 1 calc R . .
H21C H -0.5073 0.7168 0.2134 0.117 Uiso 1 1 calc R . .
C22 C -0.3867(3) 0.8271(2) 0.3433(3) 0.0798(12) Uani 1 1 d . . .
H22A H -0.3604 0.8342 0.2953 0.120 Uiso 1 1 calc R . .
H22B H -0.3195 0.8439 0.3903 0.120 Uiso 1 1 calc R . .
H22C H -0.4560 0.8619 0.3497 0.120 Uiso 1 1 calc R . .
C23 C -0.4665(3) 0.7242(2) 0.4097(2) 0.0777(11) Uani 1 1 d . . .
H23A H -0.5390 0.7563 0.4139 0.116 Uiso 1 1 calc R . .
H23B H -0.4014 0.7444 0.4572 0.116 Uiso 1 1 calc R . .
H23C H -0.4860 0.6652 0.4060 0.116 Uiso 1 1 calc R . .
C24 C -0.1645(3) 0.14973(19) 0.24413(18) 0.0482(8) Uani 1 1 d . . .
H24A H -0.2308 0.1196 0.2019 0.072 Uiso 1 1 calc R . .
H24B H -0.1060 0.1101 0.2634 0.072 Uiso 1 1 calc R . .
H24C H -0.1237 0.1895 0.2227 0.072 Uiso 1 1 calc R . .
C25 C -0.1001(3) 0.2469(2) 0.41474(19) 0.0618(9) Uani 1 1 d . . .
H25A H -0.0482 0.2862 0.4003 0.093 Uiso 1 1 calc R . .
H25B H -0.0520 0.2006 0.4301 0.093 Uiso 1 1 calc R . .
H25C H -0.1331 0.2753 0.4598 0.093 Uiso 1 1 calc R . .
C26 C -0.3376(2) 0.13747(18) 0.35432(17) 0.0402(7) Uani 1 1 d . . .
C27 C -0.4414(2) 0.1067(2) 0.28082(19) 0.0581(9) Uani 1 1 d . . .
H27A H -0.4996 0.0714 0.2948 0.087 Uiso 1 1 calc R . .
H27B H -0.4082 0.0745 0.2375 0.087 Uiso 1 1 calc R . .
H27C H -0.4826 0.1546 0.2633 0.087 Uiso 1 1 calc R . .
C28 C -0.3913(3) 0.1864(2) 0.4222(2) 0.0651(10) Uani 1 1 d . . .
H28A H -0.4330 0.2343 0.4050 0.098 Uiso 1 1 calc R . .
H28B H -0.3258 0.2059 0.4696 0.098 Uiso 1 1 calc R . .
H28C H -0.4495 0.1502 0.4351 0.098 Uiso 1 1 calc R . .
C29 C -0.2745(3) 0.0620(2) 0.3800(2) 0.0567(9) Uani 1 1 d . . .
H29A H -0.3331 0.0264 0.3932 0.085 Uiso 1 1 calc R . .
H29B H -0.2080 0.0806 0.4271 0.085 Uiso 1 1 calc R . .
H29C H -0.2416 0.0305 0.3361 0.085 Uiso 1 1 calc R . .
C30 C 0.2906(3) 0.21924(18) 0.10357(18) 0.0422(7) Uani 1 1 d . . .
C31 C 0.1626(2) 0.23415(18) 0.11461(16) 0.0394(7) Uani 1 1 d . . .
H31 H 0.1434 0.2929 0.1107 0.047 Uiso 1 1 calc R . .
C32 C 0.1423(2) 0.21957(16) 0.19499(16) 0.0344(7) Uani 1 1 d . . .
H32 H 0.0597 0.2399 0.1986 0.041 Uiso 1 1 calc R . .
C33 C 0.2280(2) 0.26006(17) 0.27387(16) 0.0382(7) Uani 1 1 d . . .
H33 H 0.3134 0.2631 0.2671 0.046 Uiso 1 1 calc R . .
C34 C 0.2161(2) 0.19995(17) 0.32860(16) 0.0409(7) Uani 1 1 d . . .
H34A H 0.2883 0.2055 0.3736 0.049 Uiso 1 1 calc R . .
H34B H 0.1426 0.2107 0.3505 0.049 Uiso 1 1 calc R . .
C35 C 0.2061(2) 0.11411(17) 0.27470(16) 0.0369(7) Uani 1 1 d . . .
H35 H 0.2893 0.0958 0.2703 0.044 Uiso 1 1 calc R . .
C36 C 0.1365(2) 0.12821(17) 0.19461(16) 0.0343(7) Uani 1 1 d . . .
C37 C 0.0677(2) 0.07625(18) 0.13290(17) 0.0393(7) Uani 1 1 d . . .
H37 H 0.0617 0.0183 0.1319 0.047 Uiso 1 1 calc R . .
C38 C -0.0002(2) 0.11260(18) 0.06464(17) 0.0415(7) Uani 1 1 d . . .
H38A H -0.0717 0.1411 0.0796 0.050 Uiso 1 1 calc R . .
H38B H -0.0301 0.0672 0.0174 0.050 Uiso 1 1 calc R . .
C39 C 0.0815(2) 0.17536(18) 0.04262(17) 0.0430(7) Uani 1 1 d . . .
H39 H 0.0288 0.2094 0.0084 0.052 Uiso 1 1 calc R . .
C40 C 0.1679(3) 0.1298(2) -0.00357(18) 0.0461(8) Uani 1 1 d . . .
C41 C 0.3916(3) 0.13541(18) 0.00232(17) 0.0433(7) Uani 1 1 d . . .
C42 C 0.4930(3) 0.11186(18) 0.05215(18) 0.0456(8) Uani 1 1 d . . .
H42 H 0.4925 0.1102 0.1060 0.055 Uiso 1 1 calc R . .
C43 C 0.5951(3) 0.09075(19) 0.02254(19) 0.0532(8) Uani 1 1 d . . .
H43 H 0.6655 0.0749 0.0565 0.064 Uiso 1 1 calc R . .
C44 C 0.5960(3) 0.0924(2) -0.0553(2) 0.0612(9) Uani 1 1 d . . .
H44 H 0.6668 0.0781 -0.0751 0.073 Uiso 1 1 calc R . .
C45 C 0.4948(3) 0.1148(2) -0.1042(2) 0.0660(10) Uani 1 1 d . . .
H45 H 0.4954 0.1154 -0.1582 0.079 Uiso 1 1 calc R . .
C46 C 0.3906(3) 0.1368(2) -0.07619(18) 0.0542(8) Uani 1 1 d . . .
H46 H 0.3204 0.1524 -0.1104 0.065 Uiso 1 1 calc R . .
C47 C 0.4035(3) 0.4142(2) 0.4170(2) 0.0762(11) Uani 1 1 d . . .
H47A H 0.3712 0.4034 0.4616 0.114 Uiso 1 1 calc R . .
H47B H 0.4556 0.4652 0.4347 0.114 Uiso 1 1 calc R . .
H47C H 0.4512 0.3673 0.3987 0.114 Uiso 1 1 calc R . .
C48 C 0.3383(3) 0.4515(2) 0.2513(2) 0.0643(10) Uani 1 1 d . . .
H48A H 0.3778 0.4028 0.2273 0.097 Uiso 1 1 calc R . .
H48B H 0.3980 0.4984 0.2724 0.097 Uiso 1 1 calc R . .
H48C H 0.2720 0.4664 0.2106 0.097 Uiso 1 1 calc R . .
C49 C 0.1706(2) 0.50821(18) 0.36625(18) 0.0452(8) Uani 1 1 d . . .
C50 C 0.0708(3) 0.5172(2) 0.2937(2) 0.0694(10) Uani 1 1 d . . .
H50A H 0.0146 0.5591 0.3106 0.104 Uiso 1 1 calc R . .
H50B H 0.0261 0.4637 0.2704 0.104 Uiso 1 1 calc R . .
H50C H 0.1076 0.5347 0.2537 0.104 Uiso 1 1 calc R . .
C51 C 0.2401(3) 0.5924(2) 0.4024(2) 0.0678(10) Uani 1 1 d . . .
H51A H 0.2788 0.6090 0.3627 0.102 Uiso 1 1 calc R . .
H51B H 0.3026 0.5874 0.4498 0.102 Uiso 1 1 calc R . .
H51C H 0.1834 0.6346 0.4177 0.102 Uiso 1 1 calc R . .
C52 C 0.1109(3) 0.4831(2) 0.4286(2) 0.0812(12) Uani 1 1 d . . .
H52A H 0.0590 0.5274 0.4468 0.122 Uiso 1 1 calc R . .
H52B H 0.1740 0.4743 0.4742 0.122 Uiso 1 1 calc R . .
H52C H 0.0614 0.4315 0.4048 0.122 Uiso 1 1 calc R . .
C53 C 0.3299(3) -0.0187(2) 0.4083(2) 0.0626(9) Uani 1 1 d . . .
H53A H 0.3965 0.0136 0.3992 0.094 Uiso 1 1 calc R . .
H53B H 0.3590 -0.0725 0.4190 0.094 Uiso 1 1 calc R . .
H53C H 0.3013 0.0121 0.4543 0.094 Uiso 1 1 calc R . .
C54 C 0.2597(3) -0.0879(2) 0.2293(2) 0.0675(10) Uani 1 1 d . . .
H54A H 0.1927 -0.0972 0.1816 0.101 Uiso 1 1 calc R . .
H54B H 0.2926 -0.1415 0.2378 0.101 Uiso 1 1 calc R . .
H54C H 0.3239 -0.0524 0.2217 0.101 Uiso 1 1 calc R . .
C55 C 0.0717(3) -0.09711(19) 0.33102(19) 0.0493(8) Uani 1 1 d . . .
C56 C 0.0263(3) -0.0508(2) 0.4034(2) 0.0668(10) Uani 1 1 d . . .
H56A H -0.0437 -0.0820 0.4094 0.100 Uiso 1 1 calc R . .
H56B H 0.0021 0.0047 0.3953 0.100 Uiso 1 1 calc R . .
H56C H 0.0915 -0.0456 0.4518 0.100 Uiso 1 1 calc R . .
C57 C -0.0335(3) -0.1055(2) 0.2564(2) 0.0732(11) Uani 1 1 d . . .
H57A H -0.0068 -0.1361 0.2095 0.110 Uiso 1 1 calc R . .
H57B H -0.0575 -0.0500 0.2480 0.110 Uiso 1 1 calc R . .
H57C H -0.1030 -0.1358 0.2642 0.110 Uiso 1 1 calc R . .
C58 C 0.1116(3) -0.1841(2) 0.3440(2) 0.0748(11) Uani 1 1 d . . .
H58A H 0.1781 -0.1782 0.3917 0.112 Uiso 1 1 calc R . .
H58B H 0.1393 -0.2139 0.2972 0.112 Uiso 1 1 calc R . .
H58C H 0.0427 -0.2154 0.3513 0.112 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 0.0434(5) 0.0360(5) 0.0508(5) 0.0072(4) 0.0169(4) 0.0015(4)
Si2 0.0335(4) 0.0386(5) 0.0417(5) 0.0125(4) 0.0096(4) 0.0056(4)
Si3 0.0368(4) 0.0353(5) 0.0464(5) 0.0037(4) 0.0074(4) -0.0004(4)
Si4 0.0434(5) 0.0410(5) 0.0481(5) 0.0168(4) 0.0158(4) 0.0085(4)
O1 0.0422(10) 0.0299(11) 0.0534(13) 0.0061(9) 0.0181(9) 0.0040(9)
O2 0.0629(14) 0.112(2) 0.0430(14) 0.0328(14) 0.0118(11) 0.0292(14)
O3 0.0451(12) 0.0900(18) 0.0649(15) 0.0469(13) 0.0233(11) 0.0293(12)
O4 0.0369(10) 0.0403(12) 0.0617(13) 0.0224(10) 0.0162(9) 0.0083(9)
O5 0.0348(10) 0.0328(12) 0.0585(13) -0.0003(10) 0.0119(9) -0.0001(9)
O6 0.0383(10) 0.0374(12) 0.0480(12) 0.0156(9) 0.0174(9) 0.0051(9)
O7 0.0627(14) 0.0860(18) 0.0423(14) -0.0098(13) 0.0146(11) -0.0257(13)
O8 0.0454(12) 0.0627(15) 0.0565(14) -0.0154(12) 0.0172(11) -0.0173(11)
N1 0.0448(14) 0.0444(16) 0.0369(14) 0.0117(12) 0.0134(11) 0.0129(11)
N2 0.0421(14) 0.0420(15) 0.0337(14) 0.0037(12) 0.0103(11) -0.0062(11)
C1 0.0498(19) 0.054(2) 0.039(2) 0.0066(16) 0.0076(15) 0.0115(16)
C2 0.0427(16) 0.0415(19) 0.0486(19) 0.0043(15) 0.0033(14) 0.0011(14)
C3 0.0373(15) 0.047(2) 0.0505(19) 0.0137(16) 0.0041(14) 0.0005(14)
C4 0.0372(15) 0.0351(18) 0.052(2) 0.0099(15) 0.0136(15) 0.0034(14)
C5 0.0304(14) 0.0395(19) 0.0423(18) 0.0118(15) 0.0129(13) 0.0035(13)
C6 0.0338(14) 0.0312(17) 0.0498(19) 0.0043(14) 0.0142(14) 0.0037(13)
C7 0.0388(15) 0.0411(19) 0.0460(18) 0.0115(15) 0.0099(13) 0.0045(13)
C8 0.0317(14) 0.0365(18) 0.0498(19) 0.0143(15) 0.0124(13) 0.0050(13)
C9 0.0297(14) 0.0300(17) 0.0463(18) 0.0082(14) 0.0097(13) 0.0015(12)
C10 0.0438(16) 0.0329(17) 0.0516(19) 0.0090(15) 0.0106(14) 0.0014(13)
C11 0.0518(19) 0.0374(18) 0.047(2) 0.0135(15) 0.0163(16) 0.0104(15)
C12 0.0549(19) 0.0415(19) 0.0411(19) 0.0166(15) 0.0189(16) 0.0166(15)
C13 0.0530(19) 0.049(2) 0.0460(19) 0.0213(16) 0.0177(16) 0.0164(16)
C14 0.0542(19) 0.057(2) 0.061(2) 0.0282(18) 0.0198(17) 0.0123(16)
C15 0.067(2) 0.076(3) 0.068(3) 0.031(2) 0.039(2) 0.022(2)
C16 0.086(3) 0.067(3) 0.052(2) 0.0178(19) 0.034(2) 0.018(2)
C17 0.072(2) 0.052(2) 0.047(2) 0.0115(17) 0.0220(18) 0.0118(17)
C18 0.0493(18) 0.061(2) 0.077(3) 0.006(2) 0.0006(17) -0.0010(17)
C19 0.084(2) 0.055(2) 0.076(3) 0.0109(19) 0.043(2) -0.0068(19)
C20 0.0517(18) 0.0367(19) 0.062(2) 0.0074(16) 0.0157(16) 0.0059(15)
C21 0.063(2) 0.058(2) 0.102(3) 0.018(2) -0.004(2) 0.0129(19)
C22 0.076(2) 0.039(2) 0.124(4) 0.012(2) 0.027(2) 0.0150(18)
C23 0.072(2) 0.079(3) 0.091(3) 0.009(2) 0.047(2) 0.018(2)
C24 0.0495(17) 0.0448(19) 0.057(2) 0.0151(16) 0.0221(15) 0.0064(15)
C25 0.0489(18) 0.070(2) 0.060(2) 0.0064(18) 0.0040(16) 0.0026(17)
C26 0.0385(15) 0.0435(19) 0.0447(18) 0.0186(15) 0.0139(14) 0.0085(14)
C27 0.0409(17) 0.066(2) 0.071(2) 0.0296(19) 0.0070(16) -0.0042(16)
C28 0.074(2) 0.064(2) 0.074(3) 0.0222(19) 0.046(2) 0.0137(18)
C29 0.0551(19) 0.056(2) 0.069(2) 0.0335(18) 0.0169(17) 0.0089(16)
C30 0.0450(18) 0.0367(18) 0.0452(19) 0.0069(15) 0.0119(15) -0.0061(15)
C31 0.0410(16) 0.0334(17) 0.0447(18) 0.0099(14) 0.0103(14) 0.0028(13)
C32 0.0287(14) 0.0318(17) 0.0426(17) 0.0077(13) 0.0078(12) 0.0012(12)
C33 0.0334(15) 0.0336(18) 0.0458(18) 0.0028(14) 0.0100(13) 0.0022(13)
C34 0.0385(15) 0.0421(19) 0.0405(18) 0.0070(15) 0.0065(13) 0.0000(13)
C35 0.0311(14) 0.0360(18) 0.0451(18) 0.0118(14) 0.0086(13) 0.0037(13)
C36 0.0293(14) 0.0359(18) 0.0391(18) 0.0076(14) 0.0112(13) 0.0038(13)
C37 0.0372(15) 0.0358(18) 0.0471(19) 0.0100(15) 0.0126(14) 0.0009(14)
C38 0.0342(15) 0.0395(18) 0.0484(19) 0.0073(15) 0.0057(13) -0.0003(13)
C39 0.0404(16) 0.0420(19) 0.0460(19) 0.0164(15) 0.0024(14) -0.0004(14)
C40 0.0509(19) 0.051(2) 0.0346(19) 0.0084(17) 0.0069(15) -0.0090(16)
C41 0.0495(18) 0.0389(18) 0.0416(19) 0.0008(14) 0.0174(15) -0.0097(14)
C42 0.0514(18) 0.0434(19) 0.0424(18) 0.0020(15) 0.0177(16) -0.0024(15)
C43 0.0560(19) 0.050(2) 0.050(2) 0.0002(16) 0.0146(17) -0.0026(16)
C44 0.059(2) 0.064(2) 0.063(3) 0.0030(19) 0.0291(19) 0.0001(18)
C45 0.088(3) 0.069(3) 0.050(2) 0.0088(19) 0.037(2) 0.000(2)
C46 0.063(2) 0.059(2) 0.042(2) 0.0112(16) 0.0155(17) -0.0030(17)
C47 0.062(2) 0.063(3) 0.086(3) 0.012(2) -0.017(2) -0.0013(19)
C48 0.067(2) 0.049(2) 0.087(3) 0.0068(19) 0.046(2) 0.0035(17)
C49 0.0493(17) 0.0368(18) 0.0496(19) 0.0001(15) 0.0198(15) -0.0016(14)
C50 0.0496(19) 0.063(2) 0.091(3) 0.006(2) 0.0146(19) 0.0175(17)
C51 0.063(2) 0.044(2) 0.093(3) -0.0052(19) 0.027(2) 0.0011(17)
C52 0.108(3) 0.063(3) 0.086(3) 0.002(2) 0.064(2) -0.003(2)
C53 0.0447(18) 0.075(3) 0.074(2) 0.035(2) 0.0074(17) 0.0035(17)
C54 0.092(2) 0.056(2) 0.071(2) 0.0224(19) 0.045(2) 0.0273(19)
C55 0.0495(17) 0.045(2) 0.057(2) 0.0235(16) 0.0075(16) 0.0022(15)
C56 0.0549(19) 0.086(3) 0.073(3) 0.031(2) 0.0310(18) 0.0103(19)
C57 0.065(2) 0.063(3) 0.086(3) 0.026(2) -0.005(2) -0.0140(19)
C58 0.073(2) 0.055(2) 0.106(3) 0.042(2) 0.019(2) 0.0033(19)

_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 1.6482(19) . ?
Si1 C18 1.853(3) . ?
Si1 C20 1.863(3) . ?
Si1 C19 1.866(3) . ?
Si2 O4 1.6388(19) . ?
Si2 C24 1.849(3) . ?
Si2 C25 1.852(3) . ?
Si2 C26 1.880(3) . ?
Si3 O5 1.6439(19) . ?
Si3 C47 1.847(3) . ?
Si3 C48 1.856(3) . ?
Si3 C49 1.875(3) . ?
Si4 O6 1.6426(19) . ?
Si4 C54 1.858(3) . ?
Si4 C53 1.861(3) . ?
Si4 C55 1.871(3) . ?
O1 C6 1.428(3) . ?
O2 C1 1.199(3) . ?
O3 C11 1.205(3) . ?
O4 C8 1.436(3) . ?
O5 C33 1.424(3) . ?
O6 C35 1.430(3) . ?
O7 C40 1.202(3) . ?
O8 C30 1.206(3) . ?
N1 C11 1.399(4) . ?
N1 C1 1.400(3) . ?
N1 C12 1.444(3) . ?
N2 C40 1.392(3) . ?
N2 C30 1.394(4) . ?
N2 C41 1.442(3) . ?
C1 C2 1.520(4) . ?
C2 C3 1.540(4) . ?
C2 C10 1.541(4) . ?
C3 C4 1.499(4) . ?
C4 C5 1.327(4) . ?
C5 C9 1.495(4) . ?
C5 C6 1.510(4) . ?
C6 C7 1.524(4) . ?
C7 C8 1.524(4) . ?
C8 C9 1.527(4) . ?
C9 C10 1.533(4) . ?
C10 C11 1.511(4) . ?
C12 C13 1.376(4) . ?
C12 C17 1.385(4) . ?
C13 C14 1.390(4) . ?
C14 C15 1.369(4) . ?
C15 C16 1.369(5) . ?
C16 C17 1.386(4) . ?
C20 C23 1.532(4) . ?
C20 C21 1.541(4) . ?
C20 C22 1.546(4) . ?
C26 C29 1.524(4) . ?
C26 C27 1.534(4) . ?
C26 C28 1.535(4) . ?
C30 C31 1.513(4) . ?
C31 C39 1.536(4) . ?
C31 C32 1.541(4) . ?
C32 C36 1.500(4) . ?
C32 C33 1.525(4) . ?
C33 C34 1.534(4) . ?
C34 C35 1.518(4) . ?
C35 C36 1.510(4) . ?
C36 C37 1.325(4) . ?
C37 C38 1.501(4) . ?
C38 C39 1.546(4) . ?
C39 C40 1.506(4) . ?
C41 C46 1.378(4) . ?
C41 C42 1.382(4) . ?
C42 C43 1.383(4) . ?
C43 C44 1.372(4) . ?
C44 C45 1.365(4) . ?
C45 C46 1.393(4) . ?
C49 C52 1.526(4) . ?
C49 C50 1.531(4) . ?
C49 C51 1.537(4) . ?
C55 C56 1.531(4) . ?
C55 C58 1.541(4) . ?
C55 C57 1.541(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Si1 C18 110.19(14) . . ?
O1 Si1 C20 104.92(11) . . ?
C18 Si1 C20 111.07(15) . . ?
O1 Si1 C19 109.42(13) . . ?
C18 Si1 C19 109.81(16) . . ?
C20 Si1 C19 111.32(15) . . ?
O4 Si2 C24 110.93(12) . . ?
O4 Si2 C25 110.19(13) . . ?
C24 Si2 C25 109.35(14) . . ?
O4 Si2 C26 103.68(11) . . ?
C24 Si2 C26 110.93(13) . . ?
C25 Si2 C26 111.67(14) . . ?
O5 Si3 C47 109.73(14) . . ?
O5 Si3 C48 110.56(13) . . ?
C47 Si3 C48 109.18(17) . . ?
O5 Si3 C49 103.85(11) . . ?
C47 Si3 C49 112.51(16) . . ?
C48 Si3 C49 110.92(14) . . ?
O6 Si4 C54 109.38(12) . . ?
O6 Si4 C53 109.92(14) . . ?
C54 Si4 C53 109.39(16) . . ?
O6 Si4 C55 104.64(11) . . ?
C54 Si4 C55 111.60(15) . . ?
C53 Si4 C55 111.81(14) . . ?
C6 O1 Si1 124.65(15) . . ?
C8 O4 Si2 127.19(15) . . ?
C33 O5 Si3 126.13(15) . . ?
C35 O6 Si4 124.82(15) . . ?
C11 N1 C1 112.5(2) . . ?
C11 N1 C12 123.0(2) . . ?
C1 N1 C12 124.5(2) . . ?
C40 N2 C30 112.1(2) . . ?
C40 N2 C41 124.3(2) . . ?
C30 N2 C41 123.6(2) . . ?
O2 C1 N1 124.1(3) . . ?
O2 C1 C2 127.5(3) . . ?
N1 C1 C2 108.3(3) . . ?
C1 C2 C3 109.9(2) . . ?
C1 C2 C10 105.2(2) . . ?
C3 C2 C10 114.8(2) . . ?
C4 C3 C2 111.3(2) . . ?
C5 C4 C3 117.3(3) . . ?
C4 C5 C9 119.8(3) . . ?
C4 C5 C6 130.7(3) . . ?
C9 C5 C6 109.2(2) . . ?
O1 C6 C5 113.0(2) . . ?
O1 C6 C7 112.6(2) . . ?
C5 C6 C7 103.2(2) . . ?
C6 C7 C8 104.5(2) . . ?
O4 C8 C7 111.6(2) . . ?
O4 C8 C9 110.4(2) . . ?
C7 C8 C9 103.5(2) . . ?
C5 C9 C8 105.7(2) . . ?
C5 C9 C10 110.8(2) . . ?
C8 C9 C10 120.9(2) . . ?
C11 C10 C9 113.9(2) . . ?
C11 C10 C2 104.8(2) . . ?
C9 C10 C2 111.8(2) . . ?
O3 C11 N1 123.0(3) . . ?
O3 C11 C10 127.9(3) . . ?
N1 C11 C10 109.1(2) . . ?
C13 C12 C17 120.9(3) . . ?
C13 C12 N1 119.9(3) . . ?
C17 C12 N1 119.2(3) . . ?
C12 C13 C14 119.2(3) . . ?
C15 C14 C13 120.2(3) . . ?
C16 C15 C14 120.3(3) . . ?
C15 C16 C17 120.6(3) . . ?
C12 C17 C16 118.8(3) . . ?
C23 C20 C21 108.4(3) . . ?
C23 C20 C22 109.3(3) . . ?
C21 C20 C22 109.5(3) . . ?
C23 C20 Si1 109.9(2) . . ?
C21 C20 Si1 109.8(2) . . ?
C22 C20 Si1 109.9(2) . . ?
C29 C26 C27 108.4(3) . . ?
C29 C26 C28 109.8(2) . . ?
C27 C26 C28 108.8(2) . . ?
C29 C26 Si2 110.16(18) . . ?
C27 C26 Si2 109.48(19) . . ?
C28 C26 Si2 110.1(2) . . ?
O8 C30 N2 123.2(3) . . ?
O8 C30 C31 127.6(3) . . ?
N2 C30 C31 109.2(2) . . ?
C30 C31 C39 104.5(2) . . ?
C30 C31 C32 114.0(2) . . ?
C39 C31 C32 112.3(2) . . ?
C36 C32 C33 106.1(2) . . ?
C36 C32 C31 110.6(2) . . ?
C33 C32 C31 120.9(2) . . ?
O5 C33 C32 110.3(2) . . ?
O5 C33 C34 111.8(2) . . ?
C32 C33 C34 102.8(2) . . ?
C35 C34 C33 104.5(2) . . ?
O6 C35 C36 112.5(2) . . ?
O6 C35 C34 112.8(2) . . ?
C36 C35 C34 103.5(2) . . ?
C37 C36 C32 120.0(2) . . ?
C37 C36 C35 130.8(3) . . ?
C32 C36 C35 108.8(2) . . ?
C36 C37 C38 117.3(3) . . ?
C37 C38 C39 111.3(2) . . ?
C40 C39 C31 105.3(2) . . ?
C40 C39 C38 110.2(2) . . ?
C31 C39 C38 114.7(2) . . ?
O7 C40 N2 124.0(3) . . ?
O7 C40 C39 127.1(3) . . ?
N2 C40 C39 109.0(2) . . ?
C46 C41 C42 121.0(3) . . ?
C46 C41 N2 119.6(3) . . ?
C42 C41 N2 119.5(3) . . ?
C41 C42 C43 119.0(3) . . ?
C44 C43 C42 120.7(3) . . ?
C45 C44 C43 119.7(3) . . ?
C44 C45 C46 121.1(3) . . ?
C41 C46 C45 118.5(3) . . ?
C52 C49 C50 108.6(3) . . ?
C52 C49 C51 109.0(3) . . ?
C50 C49 C51 109.1(3) . . ?
C52 C49 Si3 110.4(2) . . ?
C50 C49 Si3 109.3(2) . . ?
C51 C49 Si3 110.41(19) . . ?
C56 C55 C58 109.7(3) . . ?
C56 C55 C57 108.1(3) . . ?
C58 C55 C57 109.9(3) . . ?
C56 C55 Si4 109.5(2) . . ?
C58 C55 Si4 110.0(2) . . ?
C57 C55 Si4 109.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        22.98
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.045
#END===