#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:02:37 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180462 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/31/7213163.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7213163
loop_
_publ_author_name
'Berry, Malcolm B.'
'Griffiths, Russell J.'
'Howard, Judith A. K.'
'Leech, Michael A.'
'Steel, Patrick G.'
'Yufit, Dmitrii S.'
_publ_section_title
;
 Reactions of acylpolysilanes with silyl Lewis acids
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              3645
_journal_paper_doi               10.1039/a906377c
_journal_year                    1999
_chemical_formula_sum            'C20 H41 F3 O2 Si5'
_chemical_formula_weight         510.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.67(3)
_cell_angle_beta                 109.10(3)
_cell_angle_gamma                90.40(3)
_cell_formula_units_Z            2
_cell_length_a                   10.237(2)
_cell_length_b                   10.977(2)
_cell_length_c                   13.598(3)
_cell_measurement_reflns_used    499
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      1.52
_cell_volume                     1415.2(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART-CCD'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15765
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         6471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0453P)²+0.7625P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                5701
_reflns_number_total             6471
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906377csup1.cif
_cod_data_source_block           ml1
_cod_original_cell_volume        1415.2(5)
_cod_database_code               7213163
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
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_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'
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_3
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) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
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)
