# Supplementary Material (ESI) for Perkin Transactions
# This journal is © The Royal Society of Chemistry 1999
# CCDC Number: 207/379
 
data_ml1 
 
_audit_creation_method            SHELXL-97 
_publ_contact_author_name         'Patrick G. Steel'
_publ_contact_author_address
;
Chemistry Department,
University of Durham,
South Rd.,
Durham
DH1 3LE
UK
;
_publ_contact_author_email        'p.g.steel@dur.ac.uk'

loop_
_publ_author_name
'Berry, Malcolm B.' 
'Griffiths, Russell J.'
'Howard, Judith A. K.'
'Leech, Michael A.'
'Steel, Patrick G.'
'Yufit, Dimitrii S.' 

_publ_section_title
;
Reactions of Acylpolysilanes with Silyl Lewis Acids
;

_publ_requested_journal 'Perkin Trans. 1'

_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C20 H41 F3 O2 Si5' 
_chemical_formula_weight          510.98 
 
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' 
 'F'  'F'   0.0171   0.0103 
 '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                    10.237(2) 
_cell_length_b                    10.977(2) 
_cell_length_c                    13.598(3) 
_cell_angle_alpha                 100.67(3) 
_cell_angle_beta                  109.10(3) 
_cell_angle_gamma                 90.40(3) 
_cell_volume                      1415.2(5) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     499 
_cell_measurement_theta_min       1.52
_cell_measurement_theta_max       26.40
 
_exptl_crystal_description        block 
_exptl_crystal_colour             Colourless
_exptl_crystal_size_max           0.69 
_exptl_crystal_size_mid           0.39
_exptl_crystal_size_min           0.23
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.199 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              548 
_exptl_absorpt_coefficient_mu     0.286 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.817 
_exptl_absorpt_correction_T_max   0.901
_exptl_absorpt_process_details    'SADABS (Sheldrick, 1996)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       120(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 SMART-CCD'
_diffrn_measurement_method        '\w-scan'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             15765 
_diffrn_reflns_av_R_equivalents   0.0228 
_diffrn_reflns_av_sigmaI/netI     0.0248 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          1.62 
_diffrn_reflns_theta_max          27.48 
_reflns_number_total              6471 
_reflns_number_gt                 5701 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Bruker SMART'
_computing_cell_refinement        'Bruker SMART'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXL-97 (Sheldrick, 1997)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0453P)^2^+0.7625P] 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          6471 
_refine_ls_number_parameters      284 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0378 
_refine_ls_R_factor_gt            0.0316 
_refine_ls_wR_factor_ref          0.0903 
_refine_ls_wR_factor_gt           0.0847 
_refine_ls_goodness_of_fit_ref    1.042 
_refine_ls_restrained_S_all       1.042 
_refine_ls_shift/su_max           0.009 
_refine_ls_shift/su_mean          0.001 
 
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 0.93547(4) 0.86105(3) 0.29017(3) 0.01474(9) Uani 1 1 d . . . 
Si2 Si 0.78591(4) 0.67972(4) 0.07943(3) 0.01718(9) Uani 1 1 d . . . 
Si3 Si 0.75055(4) 0.62848(3) 0.29215(3) 0.01645(9) Uani 1 1 d . . . 
Si4 Si 0.74219(5) 1.07727(4) 0.22177(3) 0.02404(10) Uani 1 1 d . . . 
Si5 Si 1.15420(4) 0.92787(4) 0.28259(4) 0.02415(10) Uani 1 1 d . . . 
F1 F 1.37282(10) 0.32048(9) 0.25861(8) 0.0299(2) Uani 1 1 d . . . 
F2 F 1.47999(9) 0.46908(10) 0.38916(8) 0.0315(2) Uani 1 1 d . . . 
F3 F 1.36094(11) 0.32307(10) 0.41435(9) 0.0392(3) Uani 1 1 d . . . 
O2 O 0.95056(11) 0.88832(10) 0.41831(8) 0.0216(2) Uani 1 1 d . . . 
H2 H 0.8833 0.8547 0.4255 0.032 Uiso 1 1 calc R . . 
O1 O 0.81488(11) 0.94476(9) 0.23081(8) 0.0217(2) Uani 1 1 d . . . 
C1 C 0.87681(13) 0.68966(12) 0.23030(10) 0.0136(2) Uani 1 1 d . . . 
C3 C 1.11742(15) 0.65222(13) 0.35301(11) 0.0186(3) Uani 1 1 d . . . 
H3 H 1.1159 0.7276 0.3970 0.022 Uiso 1 1 calc R . . 
C2 C 1.00188(13) 0.61114(12) 0.26089(10) 0.0144(2) Uani 1 1 d . . . 
C6 C 1.11984(15) 0.42207(13) 0.23137(11) 0.0208(3) Uani 1 1 d . . . 
H6 H 1.1186 0.3432 0.1915 0.025 Uiso 1 1 calc R . . 
C5 C 1.23594(14) 0.46948(13) 0.31826(11) 0.0174(3) Uani 1 1 d . . . 
C7 C 1.00533(15) 0.49173(13) 0.20351(11) 0.0191(3) Uani 1 1 d . . . 
H7 H 0.9286 0.4581 0.1450 0.023 Uiso 1 1 calc R . . 
C4 C 1.23318(15) 0.58459(13) 0.38057(11) 0.0196(3) Uani 1 1 d . . . 
H4 H 1.3089 0.6161 0.4406 0.024 Uiso 1 1 calc R . . 
C20 C 1.36112(16) 0.39602(14) 0.34502(12) 0.0228(3) Uani 1 1 d . . . 
C11 C 0.62065(16) 0.74136(15) 0.31198(13) 0.0261(3) Uani 1 1 d . . . 
H11A H 0.5649 0.7080 0.3467 0.039 Uiso 1 1 calc R . . 
H11B H 0.5623 0.7554 0.2443 0.039 Uiso 1 1 calc R . . 
H11C H 0.6682 0.8185 0.3550 0.039 Uiso 1 1 calc R . . 
C8 C 0.88254(17) 0.78109(15) 0.02517(12) 0.0258(3) Uani 1 1 d . . . 
H8A H 0.8274 0.7856 -0.0462 0.039 Uiso 1 1 calc R . . 
H8B H 0.9684 0.7465 0.0253 0.039 Uiso 1 1 calc R . . 
H8C H 0.9012 0.8630 0.0686 0.039 Uiso 1 1 calc R . . 
C10 C 0.76431(17) 0.52277(14) -0.01109(12) 0.0247(3) Uani 1 1 d . . . 
H10A H 0.7227 0.4628 0.0149 0.037 Uiso 1 1 calc R . . 
H10B H 0.8534 0.4979 -0.0128 0.037 Uiso 1 1 calc R . . 
H10C H 0.7059 0.5278 -0.0814 0.037 Uiso 1 1 calc R . . 
C12 C 0.65435(16) 0.47937(14) 0.20611(13) 0.0252(3) Uani 1 1 d . . . 
H12A H 0.7194 0.4217 0.1926 0.038 Uiso 1 1 calc R . . 
H12B H 0.5936 0.4958 0.1401 0.038 Uiso 1 1 calc R . . 
H12C H 0.6008 0.4445 0.2417 0.038 Uiso 1 1 calc R . . 
C9 C 0.60526(16) 0.73186(15) 0.04904(12) 0.0262(3) Uani 1 1 d . . . 
H9A H 0.6073 0.8125 0.0916 0.039 Uiso 1 1 calc R . . 
H9B H 0.5482 0.6737 0.0648 0.039 Uiso 1 1 calc R . . 
H9C H 0.5679 0.7360 -0.0248 0.039 Uiso 1 1 calc R . . 
C14 C 0.8420(2) 1.20026(16) 0.33690(15) 0.0393(4) Uani 1 1 d . . . 
H14A H 0.8562 1.1708 0.4016 0.059 Uiso 1 1 calc R . . 
H14B H 0.7910 1.2733 0.3378 0.059 Uiso 1 1 calc R . . 
H14C H 0.9301 1.2200 0.3307 0.059 Uiso 1 1 calc R . . 
C13 C 0.84870(16) 0.59111(15) 0.42414(12) 0.0247(3) Uani 1 1 d . . . 
H13A H 0.9045 0.6635 0.4697 0.037 Uiso 1 1 calc R . . 
H13B H 0.9074 0.5252 0.4148 0.037 Uiso 1 1 calc R . . 
H13C H 0.7846 0.5654 0.4557 0.037 Uiso 1 1 calc R . . 
C15 C 0.7392(2) 1.11769(18) 0.09380(15) 0.0407(4) Uani 1 1 d . . . 
H15A H 0.8325 1.1335 0.0957 0.061 Uiso 1 1 calc R . . 
H15B H 0.6894 1.1906 0.0834 0.061 Uiso 1 1 calc R . . 
H15C H 0.6943 1.0498 0.0364 0.061 Uiso 1 1 calc R . . 
C19 C 1.23566(18) 0.81276(18) 0.20417(15) 0.0351(4) Uani 1 1 d . . . 
H19A H 1.1933 0.8127 0.1299 0.053 Uiso 1 1 calc R . . 
H19B H 1.2222 0.7313 0.2171 0.053 Uiso 1 1 calc R . . 
H19C H 1.3331 0.8355 0.2255 0.053 Uiso 1 1 calc R . . 
C18 C 1.2791(2) 0.9738(2) 0.42193(17) 0.0489(5) Uani 1 1 d . . . 
H18A H 1.2969 0.9018 0.4537 0.073 Uiso 1 1 calc R . . 
H18B H 1.2399 1.0341 0.4628 0.073 Uiso 1 1 calc R . . 
H18C H 1.3644 1.0091 0.4205 0.073 Uiso 1 1 calc R . . 
C16 C 0.5624(2) 1.05763(19) 0.22356(19) 0.0444(5) Uani 1 1 d . . . 
H16A H 0.5108 0.9930 0.1654 0.067 Uiso 1 1 calc R . . 
H16B H 0.5185 1.1341 0.2170 0.067 Uiso 1 1 calc R . . 
H16C H 0.5650 1.0356 0.2893 0.067 Uiso 1 1 calc R . . 
C17 C 1.1337(2) 1.06929(19) 0.2209(2) 0.0509(6) Uani 1 1 d . . . 
H17A H 1.2212 1.0958 0.2170 0.076 Uiso 1 1 calc R . . 
H17B H 1.1029 1.1349 0.2635 0.076 Uiso 1 1 calc R . . 
H17C H 1.0667 1.0495 0.1507 0.076 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 0.01624(18) 0.01127(17) 0.01436(17) 0.00126(13) 0.00271(13) 0.00060(13) 
Si2 0.01939(19) 0.01619(18) 0.01277(17) 0.00135(14) 0.00198(14) 0.00083(14) 
Si3 0.01620(18) 0.01561(18) 0.01711(18) 0.00184(14) 0.00577(14) -0.00004(13) 
Si4 0.0267(2) 0.0169(2) 0.0220(2) 0.00191(16) 0.00047(16) 0.00717(16) 
Si5 0.0190(2) 0.0226(2) 0.0293(2) 0.00567(17) 0.00581(16) -0.00285(15) 
F1 0.0276(5) 0.0293(5) 0.0323(5) -0.0003(4) 0.0127(4) 0.0120(4) 
F2 0.0184(4) 0.0380(5) 0.0333(5) 0.0017(4) 0.0051(4) 0.0056(4) 
F3 0.0420(6) 0.0437(6) 0.0466(6) 0.0311(5) 0.0222(5) 0.0238(5) 
O2 0.0253(5) 0.0207(5) 0.0172(5) 0.0012(4) 0.0063(4) 0.0011(4) 
O1 0.0221(5) 0.0153(5) 0.0235(5) 0.0033(4) 0.0022(4) 0.0047(4) 
C1 0.0152(6) 0.0113(6) 0.0128(6) 0.0009(4) 0.0035(5) 0.0006(4) 
C3 0.0215(7) 0.0141(6) 0.0166(6) 0.0003(5) 0.0032(5) 0.0019(5) 
C2 0.0166(6) 0.0132(6) 0.0145(6) 0.0034(5) 0.0066(5) 0.0007(5) 
C6 0.0248(7) 0.0165(6) 0.0196(7) -0.0001(5) 0.0075(6) 0.0049(5) 
C5 0.0189(6) 0.0185(6) 0.0182(6) 0.0068(5) 0.0088(5) 0.0050(5) 
C7 0.0194(6) 0.0165(6) 0.0168(6) -0.0012(5) 0.0023(5) 0.0008(5) 
C4 0.0192(6) 0.0181(7) 0.0178(6) 0.0028(5) 0.0016(5) 0.0015(5) 
C20 0.0228(7) 0.0242(7) 0.0232(7) 0.0069(6) 0.0088(6) 0.0074(6) 
C11 0.0222(7) 0.0273(8) 0.0304(8) 0.0032(6) 0.0122(6) 0.0054(6) 
C8 0.0347(8) 0.0248(7) 0.0173(7) 0.0046(6) 0.0076(6) -0.0029(6) 
C10 0.0318(8) 0.0210(7) 0.0164(7) -0.0007(5) 0.0041(6) 0.0004(6) 
C12 0.0249(7) 0.0214(7) 0.0284(8) 0.0009(6) 0.0099(6) -0.0065(6) 
C9 0.0220(7) 0.0257(8) 0.0224(7) 0.0019(6) -0.0022(6) 0.0033(6) 
C14 0.0542(11) 0.0219(8) 0.0288(9) -0.0011(7) -0.0001(8) 0.0049(8) 
C13 0.0272(8) 0.0290(8) 0.0199(7) 0.0086(6) 0.0087(6) -0.0002(6) 
C15 0.0539(12) 0.0355(10) 0.0284(9) 0.0125(8) 0.0042(8) 0.0170(8) 
C19 0.0253(8) 0.0444(10) 0.0398(10) 0.0096(8) 0.0156(7) 0.0030(7) 
C18 0.0312(10) 0.0642(14) 0.0389(11) -0.0063(10) 0.0047(8) -0.0189(9) 
C16 0.0330(10) 0.0351(10) 0.0629(13) 0.0050(9) 0.0156(9) 0.0168(8) 
C17 0.0390(11) 0.0360(11) 0.0859(17) 0.0316(11) 0.0211(11) -0.0024(8) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Si1 O1 1.6304(12) . ? 
Si1 O2 1.6672(11) . ? 
Si1 C1 1.9131(15) . ? 
Si1 Si5 2.3913(8) . ? 
Si2 C9 1.8763(16) . ? 
Si2 C8 1.8783(16) . ? 
Si2 C10 1.8877(16) . ? 
Si2 C1 1.9372(15) . ? 
Si3 C13 1.8701(16) . ? 
Si3 C11 1.8736(16) . ? 
Si3 C12 1.8793(17) . ? 
Si3 C1 1.9332(14) . ? 
Si4 O1 1.6449(11) . ? 
Si4 C16 1.861(2) . ? 
Si4 C14 1.862(2) . ? 
Si4 C15 1.865(2) . ? 
Si5 C19 1.8780(19) . ? 
Si5 C17 1.879(2) . ? 
Si5 C18 1.879(2) . ? 
F1 C20 1.3473(18) . ? 
F2 C20 1.3469(19) . ? 
F3 C20 1.3456(18) . ? 
C1 C2 1.5346(18) . ? 
C3 C4 1.386(2) . ? 
C3 C2 1.409(2) . ? 
C2 C7 1.4029(19) . ? 
C6 C5 1.387(2) . ? 
C6 C7 1.390(2) . ? 
C5 C4 1.391(2) . ? 
C5 C20 1.497(2) . ? 
 
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 O2 107.72(6) . . ? 
O1 Si1 C1 108.18(6) . . ? 
O2 Si1 C1 108.95(6) . . ? 
O1 Si1 Si5 110.07(5) . . ? 
O2 Si1 Si5 106.34(5) . . ? 
C1 Si1 Si5 115.33(5) . . ? 
C9 Si2 C8 106.94(8) . . ? 
C9 Si2 C10 104.15(8) . . ? 
C8 Si2 C10 103.88(7) . . ? 
C9 Si2 C1 111.80(7) . . ? 
C8 Si2 C1 111.39(7) . . ? 
C10 Si2 C1 117.79(7) . . ? 
C13 Si3 C11 107.81(8) . .. ? 
C13 Si3 C12 106.38(8) . . ? 
C11 Si3 C12 108.42(8) . . ? 
C13 Si3 C1 110.34(7) . . ? 
C11 Si3 C1 113.41(7) . . ? 
C12 Si3 C1 110.20(7) . . ? 
O1 Si4 C16 108.89(8) . . ? 
O1 Si4 C14 109.83(8) . . ? 
C16 Si4 C14 108.90(10) . . ? 
O1 Si4 C15 107.81(8) . . ? 
C16 Si4 C15 110.17(11) . . ? 
C14 Si4 C15 111.19(10) . . ? 
C19 Si5 C17 106.23(10) . . ? 
C19 Si5 C18 108.36(10) . . ? 
C17 Si5 C18 107.69(12) . . ? 
C19 Si5 Si1 116.39(7) . . ? 
C17 Si5 Si1 109.29(7) . . ? 
C18 Si5 Si1 108.56(7) . . ? 
Si1 O1 Si4 151.81(7) . . ? 
C2 C1 Si1 109.19(9) . . ? 
C2 C1 Si3 104.02(8) . . ? 
Si1 C1 Si3 111.38(7) . . ? 
C2 C1 Si2 115.67(9) . . ? 
Si1 C1 Si2 106.29(7) . . ? 
Si3 C1 Si2 110.38(7) . . ? 
C4 C3 C2 122.49(13) . . ? 
C7 C2 C3 115.77(13) . . ? 
C7 C2 C1 122.63(12) . . ? 
C3 C2 C1 121.48(12) . . ? 
C5 C6 C7 120.38(13) . . ? 
C6 C5 C4 119.09(13) . . ? 
C6 C5 C20 120.03(13) . . ? 
C4 C5 C20 120.87(13) . . ? 
C6 C7 C2 122.08(13) . . ? 
C3 C4 C5 119.90(13) . . ? 
F3 C20 F2 105.94(13) . . ? 
F3 C20 F1 106.35(13) . . ? 
F2 C20 F1 106.22(12) . . ? 
F3 C20 C5 113.18(12) . . ? 
F2 C20 C5 112.44(13) . . ? 
F1 C20 C5 112.18(12) . . ? 
 
_diffrn_measured_fraction_theta_max    0.993 
_diffrn_reflns_theta_full              27.48 
_diffrn_measured_fraction_theta_full   0.993 
_refine_diff_density_max    0.611 
_refine_diff_density_min   -0.500 
_refine_diff_density_rms    0.053