# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Sarah Masters' _publ_contact_author_email S.MASTERS@ED.AC.UK _publ_section_title ; The gas-phase structure of octaphenyloctasilsesquioxane (Si8O12Ph8) and the crystal structures of Si8O12(p-tolyl)8 and Si8O12(p-ClCH2C6H4)8 ; loop_ _publ_author_name 'Sarah Masters' 'Sophie Arrowsmith' 'David B. Cordes' 'Georgiy V. Girichev' 'P. Lickiss' ; S.A.Shlykov ; 'Derek A. Wann' 'Andrew J.P. White' 'Alexander V. Zakharov' # Attachment 'Dalton_10-09.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 746535' #TrackingRef 'Dalton_10-09.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H56 O12 Si8, 6(C3 H6 O)' _chemical_formula_sum 'C74 H92 O18 Si8' _chemical_formula_weight 1494.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 19.4815(3) _cell_length_b 19.4815(3) _cell_length_c 20.9445(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7949.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4372 _cell_measurement_theta_min 3.0898 _cell_measurement_theta_max 70.8155 _exptl_crystal_description needles _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3168 _exptl_absorpt_coefficient_mu 1.809 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.794 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11196 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 70.96 _reflns_number_total 3830 _reflns_number_gt 2579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1169P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3830 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1813 _refine_ls_wR_factor_gt 0.1699 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.63434(6) 0.03513(6) 0.5000 0.0348(3) Uani 1 2 d S . . Si2 Si 0.52802(4) 0.07409(4) 0.60556(3) 0.0357(2) Uani 1 1 d . . . Si3 Si 0.42094(6) 0.11329(6) 0.5000 0.0357(3) Uani 1 2 d S . . O1 O 0.63071(16) -0.04791(15) 0.5000 0.0460(7) Uani 1 2 d S . . O2 O 0.59620(11) 0.06341(11) 0.56296(9) 0.0457(5) Uani 1 1 d . . . O3 O 0.5000 0.0000 0.62868(13) 0.0443(7) Uani 1 2 d S . . O4 O 0.46951(12) 0.11039(11) 0.56252(10) 0.0467(6) Uani 1 1 d . . . C1 C 0.7234(2) 0.0661(2) 0.5000 0.0371(9) Uani 1 2 d S . . C2 C 0.75872(17) 0.07863(17) 0.44393(15) 0.0471(7) Uani 1 1 d . . . H2A H 0.7361 0.0710 0.4044 0.057 Uiso 1 1 calc R . . C3 C 0.82554(19) 0.10171(19) 0.44333(19) 0.0585(9) Uani 1 1 d . . . H3A H 0.8480 0.1099 0.4038 0.070 Uiso 1 1 calc R . . C4 C 0.8601(3) 0.1130(3) 0.5000 0.0567(13) Uani 1 2 d S . . C5 C 0.9330(3) 0.1378(4) 0.5000 0.084(2) Uani 1 2 d S . . H5A H 0.9349 0.1844 0.4824 0.126 Uiso 0.50 1 calc PR . . H5B H 0.9611 0.1071 0.4738 0.126 Uiso 0.50 1 calc PR . . H5C H 0.9506 0.1382 0.5438 0.126 Uiso 0.50 1 calc PR . . C6 C 0.55004(17) 0.12717(16) 0.67507(13) 0.0423(7) Uani 1 1 d . . . C7 C 0.6123(2) 0.1624(2) 0.67807(18) 0.0647(11) Uani 1 1 d . . . H7A H 0.6436 0.1601 0.6433 0.078 Uiso 1 1 calc R . . C8 C 0.6289(3) 0.2013(3) 0.7324(2) 0.0885(16) Uani 1 1 d . . . H8A H 0.6714 0.2251 0.7341 0.106 Uiso 1 1 calc R . . C9 C 0.5835(3) 0.2056(3) 0.78390(18) 0.0797(13) Uani 1 1 d . . . C10 C 0.5247(2) 0.1695(2) 0.78089(17) 0.0711(12) Uani 1 1 d . . . H10A H 0.4946 0.1699 0.8165 0.085 Uiso 1 1 calc R . . C11 C 0.5068(2) 0.13174(19) 0.72752(15) 0.0566(9) Uani 1 1 d . . . H11A H 0.4640 0.1084 0.7268 0.068 Uiso 1 1 calc R . . C12 C 0.6028(3) 0.2472(3) 0.8421(2) 0.123(2) Uani 1 1 d . . . H12A H 0.6202 0.2165 0.8754 0.184 Uiso 1 1 calc R . . H12B H 0.5623 0.2717 0.8579 0.184 Uiso 1 1 calc R . . H12C H 0.6385 0.2804 0.8306 0.184 Uiso 1 1 calc R . . C13 C 0.3717(2) 0.1937(2) 0.5000 0.0434(10) Uani 1 2 d S . . C14 C 0.4056(3) 0.2567(3) 0.5000 0.101(3) Uani 1 2 d S . . H14A H 0.4543 0.2578 0.5000 0.121 Uiso 1 2 calc SR . . C15 C 0.3690(4) 0.3181(3) 0.5000 0.121(4) Uani 1 2 d S . . H15A H 0.3933 0.3604 0.5000 0.145 Uiso 1 2 calc SR . . C16 C 0.2980(3) 0.3188(3) 0.5000 0.0692(16) Uani 1 2 d S . . C17 C 0.2654(3) 0.2581(3) 0.5000 0.0730(17) Uani 1 2 d S . . H17A H 0.2167 0.2576 0.5000 0.088 Uiso 1 2 calc SR . . C18 C 0.3007(3) 0.1958(3) 0.5000 0.0613(14) Uani 1 2 d S . . H18A H 0.2755 0.1541 0.5000 0.074 Uiso 1 2 calc SR . . C19 C 0.2585(4) 0.3866(3) 0.5000 0.103(3) Uani 1 2 d S . . H19A H 0.2139 0.3800 0.4793 0.155 Uiso 0.50 1 calc PR . . H19B H 0.2848 0.4213 0.4766 0.155 Uiso 0.50 1 calc PR . . H19C H 0.2516 0.4019 0.5441 0.155 Uiso 0.50 1 calc PR . . 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 0.0362(6) 0.0365(6) 0.0318(5) 0.000 0.000 -0.0020(5) Si2 0.0389(4) 0.0383(5) 0.0298(4) -0.0019(3) -0.0001(3) -0.0019(3) Si3 0.0370(6) 0.0359(6) 0.0342(5) 0.000 0.000 0.0007(5) O1 0.0477(18) 0.0374(16) 0.0529(17) 0.000 0.000 -0.0027(14) O2 0.0453(12) 0.0529(13) 0.0388(11) -0.0084(10) 0.0056(9) -0.0060(10) O3 0.0567(19) 0.0418(17) 0.0346(14) 0.000 0.000 -0.0081(14) O4 0.0533(13) 0.0454(12) 0.0415(11) -0.0019(9) -0.0094(10) 0.0019(10) C1 0.037(2) 0.033(2) 0.041(2) 0.000 0.000 -0.0003(17) C2 0.0453(18) 0.0486(19) 0.0474(17) 0.0019(15) 0.0016(15) -0.0042(15) C3 0.051(2) 0.058(2) 0.067(2) 0.0059(18) 0.0131(18) -0.0054(17) C4 0.043(3) 0.047(3) 0.081(3) 0.000 0.000 -0.005(2) C5 0.043(3) 0.090(5) 0.118(5) 0.000 0.000 -0.010(3) C6 0.0531(19) 0.0414(16) 0.0324(14) -0.0009(13) 0.0012(13) -0.0021(14) C7 0.068(2) 0.080(3) 0.0466(19) -0.0112(18) 0.0025(18) -0.019(2) C8 0.090(3) 0.108(4) 0.068(3) -0.028(3) -0.001(2) -0.044(3) C9 0.105(4) 0.088(3) 0.046(2) -0.022(2) -0.001(2) -0.022(3) C10 0.093(3) 0.078(3) 0.0420(19) -0.0166(18) 0.013(2) -0.010(2) C11 0.069(2) 0.058(2) 0.0429(17) -0.0087(16) 0.0051(16) -0.0106(19) C12 0.163(6) 0.137(5) 0.069(3) -0.051(3) 0.004(3) -0.045(4) C13 0.043(2) 0.039(2) 0.047(2) 0.000 0.000 0.0013(19) C14 0.049(3) 0.050(3) 0.203(9) 0.000 0.000 0.002(3) C15 0.075(5) 0.044(3) 0.243(12) 0.000 0.000 -0.003(3) C16 0.061(3) 0.053(3) 0.094(4) 0.000 0.000 0.017(3) C17 0.042(3) 0.072(4) 0.106(5) 0.000 0.000 0.007(3) C18 0.043(3) 0.054(3) 0.086(4) 0.000 0.000 0.004(2) C19 0.105(6) 0.068(4) 0.137(7) 0.000 0.000 0.044(4) _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 O2 1.611(2) . ? Si1 O2 1.611(2) 10_556 ? Si1 O1 1.619(3) . ? Si1 C1 1.838(4) . ? Si2 O2 1.614(2) . ? Si2 O4 1.616(2) . ? Si2 O3 1.6173(11) . ? Si2 C6 1.836(3) . ? Si3 O4 1.617(2) 10_556 ? Si3 O4 1.617(2) . ? Si3 O1 1.623(3) 9_656 ? Si3 C13 1.837(5) . ? O1 Si3 1.623(3) 9_656 ? O3 Si2 1.6173(11) 2_655 ? C1 C2 1.382(4) 10_556 ? C1 C2 1.382(4) . ? C2 C3 1.377(5) . ? C3 C4 1.382(5) . ? C4 C3 1.382(5) 10_556 ? C4 C5 1.500(7) . ? C6 C11 1.387(4) . ? C6 C7 1.396(5) . ? C7 C8 1.404(5) . ? C8 C9 1.397(6) . ? C9 C10 1.346(6) . ? C9 C12 1.511(5) . ? C10 C11 1.382(5) . ? C13 C18 1.384(7) . ? C13 C14 1.394(7) . ? C14 C15 1.393(8) . ? C15 C16 1.383(9) . ? C16 C17 1.342(8) . ? C16 C19 1.527(8) . ? C17 C18 1.395(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Si1 O2 109.89(17) . 10_556 ? O2 Si1 O1 108.76(11) . . ? O2 Si1 O1 108.76(11) 10_556 . ? O2 Si1 C1 108.86(11) . . ? O2 Si1 C1 108.86(11) 10_556 . ? O1 Si1 C1 111.69(18) . . ? O2 Si2 O4 109.18(12) . . ? O2 Si2 O3 109.16(10) . . ? O4 Si2 O3 108.63(10) . . ? O2 Si2 C6 108.58(13) . . ? O4 Si2 C6 111.13(13) . . ? O3 Si2 C6 110.12(13) . . ? O4 Si3 O4 108.19(17) 10_556 . ? O4 Si3 O1 109.60(11) 10_556 9_656 ? O4 Si3 O1 109.60(11) . 9_656 ? O4 Si3 C13 109.62(12) 10_556 . ? O4 Si3 C13 109.62(12) . . ? O1 Si3 C13 110.19(19) 9_656 . ? Si1 O1 Si3 144.2(2) . 9_656 ? Si1 O2 Si2 151.23(15) . . ? Si2 O3 Si2 145.16(19) 2_655 . ? Si2 O4 Si3 151.64(16) . . ? C2 C1 C2 116.3(4) 10_556 . ? C2 C1 Si1 121.8(2) 10_556 . ? C2 C1 Si1 121.8(2) . . ? C3 C2 C1 122.4(3) . . ? C2 C3 C4 120.3(4) . . ? C3 C4 C3 118.4(5) . 10_556 ? C3 C4 C5 120.8(2) . . ? C3 C4 C5 120.8(2) 10_556 . ? C11 C6 C7 117.4(3) . . ? C11 C6 Si2 121.5(3) . . ? C7 C6 Si2 121.0(2) . . ? C6 C7 C8 120.1(4) . . ? C9 C8 C7 120.9(4) . . ? C10 C9 C8 118.1(4) . . ? C10 C9 C12 122.0(4) . . ? C8 C9 C12 119.8(5) . . ? C9 C10 C11 122.0(4) . . ? C10 C11 C6 121.5(4) . . ? C18 C13 C14 116.6(5) . . ? C18 C13 Si3 123.2(4) . . ? C14 C13 Si3 120.2(4) . . ? C15 C14 C13 120.9(6) . . ? C16 C15 C14 121.4(6) . . ? C17 C16 C15 117.6(5) . . ? C17 C16 C19 121.6(6) . . ? C15 C16 C19 120.8(6) . . ? C16 C17 C18 122.3(5) . . ? C13 C18 C17 121.2(5) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 68.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.632 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.065 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 1437 405 ' ' 2 0.500 0.500 0.500 1437 405 ' ' _platon_squeeze_details ; SQUEEZE suggests 809 e/cell = 50.6 e/asu. The solvents used were dcm = CH2Cl2 = 42e and acetone = C3H6O = 32e From the non-SQUEEZE version, the shape and flat electron density profile slightly favours acetone over dcm, but both are possible so the choice is somewhat arbitrary. Acetone was chosen. 1.5acetone = 48e, so solvent modelled as 1.5acetone/asu = 6acetone/cage. From SQUEEZE, asu C4.5 H9 O1.5 low, so UNIT C72 H144 O24 low, i.e. C224 H224 O48 Si32 ; #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 746536' #TrackingRef 'Dalton_10-09.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H48 Cl8 O12 Si8' _chemical_formula_sum 'C56 H48 Cl8 O12 Si8' _chemical_formula_weight 1421.26 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' Cl Cl 0.1484 0.1585 '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 12.8106(6) _cell_length_b 13.2923(6) _cell_length_c 22.1442(10) _cell_angle_alpha 76.315(4) _cell_angle_beta 75.028(4) _cell_angle_gamma 61.699(5) _cell_volume 3178.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5306 _cell_measurement_theta_min 4.1694 _cell_measurement_theta_max 26.1228 _exptl_crystal_description 'hexagonal tablets' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.909 _exptl_absorpt_correction_T_max 0.987 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16990 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.1500 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.18 _diffrn_reflns_theta_max 26.18 _reflns_number_total 10107 _reflns_number_gt 4702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0593P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10107 _refine_ls_number_parameters 777 _refine_ls_number_restraints 231 _refine_ls_R_factor_all 0.1331 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.909 _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 0.50250(13) 0.42562(13) 0.29327(7) 0.0255(4) Uani 1 1 d . . . Si2 Si 0.55073(13) 0.25272(13) 0.20193(7) 0.0248(4) Uani 1 1 d . . . Si3 Si 0.71759(14) 0.05299(13) 0.28969(7) 0.0255(4) Uani 1 1 d . . . Si4 Si 0.66623(14) 0.22784(13) 0.37694(7) 0.0248(4) Uani 1 1 d . . . Si5 Si 0.71871(13) 0.46883(12) 0.20854(7) 0.0247(4) Uani 1 1 d D . . Si6 Si 0.76572(13) 0.29164(13) 0.12233(7) 0.0245(4) Uani 1 1 d . . . Si7 Si 0.93703(13) 0.09466(13) 0.21145(7) 0.0250(4) Uani 1 1 d . . . Si8 Si 0.88645(13) 0.27380(13) 0.29384(7) 0.0242(4) Uani 1 1 d D . . Cl1 Cl 0.02173(19) 0.92141(16) 0.40989(10) 0.0868(7) Uani 1 1 d . . . Cl2 Cl 0.05991(16) 0.38481(15) 0.06129(9) 0.0690(6) Uani 1 1 d . . . Cl3 Cl 0.66823(19) -0.47208(15) 0.38210(8) 0.0735(6) Uani 1 1 d . . . Cl4 Cl 0.63738(19) 0.00507(19) 0.70427(8) 0.0791(6) Uani 1 1 d . . . Cl5 Cl 0.7050(6) 0.9990(4) 0.0319(3) 0.115(2) Uani 0.486(3) 1 d PDU A 1 Cl5' Cl 0.7461(6) 1.0069(5) 0.0901(4) 0.099(3) Uani 0.312(5) 1 d PDU A 2 Cl5" Cl 0.5802(13) 0.9969(8) 0.0175(5) 0.113(5) Uani 0.202(5) 1 d PDU A -3 Cl6 Cl 0.90081(17) 0.39651(16) -0.21233(7) 0.0648(5) Uani 1 1 d . . . Cl7 Cl 1.45594(17) -0.39624(16) 0.10418(10) 0.0799(6) Uani 1 1 d . . . Cl8 Cl 1.3608(3) 0.2194(3) 0.41851(15) 0.0691(12) Uani 0.595(4) 1 d PD A 1 Cl8' Cl 1.0640(4) 0.4419(4) 0.5038(2) 0.0662(18) Uani 0.405(4) 1 d PD A -2 O1 O 0.4961(3) 0.3486(3) 0.24886(15) 0.0302(9) Uani 1 1 d . . . O2 O 0.6257(3) 0.1273(3) 0.24004(15) 0.0286(9) Uani 1 1 d . . . O3 O 0.6731(3) 0.1217(3) 0.34963(15) 0.0277(9) Uani 1 1 d . . . O4 O 0.5506(3) 0.3451(3) 0.35682(15) 0.0279(9) Uani 1 1 d . . . O5 O 0.5943(3) 0.4785(3) 0.25437(15) 0.0277(9) Uani 1 1 d . A . O6 O 0.6409(3) 0.2799(3) 0.14155(15) 0.0313(9) Uani 1 1 d . A . O7 O 0.8519(3) 0.0367(3) 0.25601(15) 0.0301(9) Uani 1 1 d . A . O8 O 0.7841(3) 0.2462(3) 0.34404(15) 0.0297(9) Uani 1 1 d . A . O9 O 0.7441(3) 0.4036(3) 0.14982(15) 0.0286(9) Uani 1 1 d . A . O10 O 0.8690(3) 0.1777(3) 0.15419(15) 0.0296(9) Uani 1 1 d . A . O11 O 0.9595(3) 0.1692(3) 0.25090(15) 0.0296(9) Uani 1 1 d . A . O12 O 0.8282(3) 0.3931(3) 0.24824(15) 0.0293(9) Uani 1 1 d . A . C11 C 0.3549(5) 0.5404(4) 0.3197(2) 0.0260(13) Uani 1 1 d . . . C12 C 0.3033(5) 0.5428(5) 0.3831(3) 0.0369(15) Uani 1 1 d . . . H12A H 0.3453 0.4829 0.4135 0.044 Uiso 1 1 calc R . . C13 C 0.1925(6) 0.6298(5) 0.4034(3) 0.0448(16) Uani 1 1 d . . . H13A H 0.1594 0.6278 0.4470 0.054 Uiso 1 1 calc R . . C14 C 0.1291(5) 0.7201(5) 0.3607(3) 0.0378(15) Uani 1 1 d . . . C15 C 0.1793(6) 0.7203(5) 0.2983(3) 0.0488(17) Uani 1 1 d . . . H15A H 0.1381 0.7822 0.2685 0.059 Uiso 1 1 calc R . . C16 C 0.2905(5) 0.6311(5) 0.2774(3) 0.0421(16) Uani 1 1 d . . . H16A H 0.3223 0.6327 0.2336 0.050 Uiso 1 1 calc R . . C17 C 0.0087(6) 0.8150(5) 0.3828(3) 0.0584(19) Uani 1 1 d . . . H17A H -0.0370 0.7814 0.4172 0.070 Uiso 1 1 calc R . . H17B H -0.0373 0.8510 0.3476 0.070 Uiso 1 1 calc R . . C21 C 0.4289(5) 0.2527(4) 0.1714(2) 0.0246(13) Uani 1 1 d . . . C22 C 0.3292(5) 0.2479(5) 0.2104(3) 0.0416(16) Uani 1 1 d . . . H22A H 0.3210 0.2461 0.2545 0.050 Uiso 1 1 calc R . . C23 C 0.2393(6) 0.2456(5) 0.1874(3) 0.0467(17) Uani 1 1 d . . . H23A H 0.1716 0.2412 0.2159 0.056 Uiso 1 1 calc R . . C24 C 0.2472(5) 0.2495(5) 0.1244(3) 0.0348(15) Uani 1 1 d . . . C25 C 0.3468(5) 0.2558(5) 0.0840(3) 0.0407(16) Uani 1 1 d . . . H25A H 0.3535 0.2593 0.0399 0.049 Uiso 1 1 calc R . . C26 C 0.4371(5) 0.2571(5) 0.1070(3) 0.0333(15) Uani 1 1 d . . . H26A H 0.5052 0.2610 0.0785 0.040 Uiso 1 1 calc R . . C27 C 0.1482(5) 0.2474(5) 0.0997(3) 0.0440(16) Uani 1 1 d . . . H27A H 0.0960 0.2234 0.1353 0.053 Uiso 1 1 calc R . . H27B H 0.1846 0.1901 0.0698 0.053 Uiso 1 1 calc R . . C31 C 0.7204(5) -0.0896(5) 0.3218(2) 0.0267(13) Uani 1 1 d . . . C32 C 0.8102(5) -0.1907(5) 0.2985(3) 0.0413(16) Uani 1 1 d . . . H32A H 0.8672 -0.1863 0.2620 0.050 Uiso 1 1 calc R . . C33 C 0.8168(6) -0.2970(5) 0.3280(3) 0.0506(18) Uani 1 1 d . . . H33A H 0.8783 -0.3647 0.3112 0.061 Uiso 1 1 calc R . . C34 C 0.7351(6) -0.3072(5) 0.3820(3) 0.0407(16) Uani 1 1 d . . . C35 C 0.6454(5) -0.2069(5) 0.4043(3) 0.0441(16) Uani 1 1 d . . . H35A H 0.5878 -0.2112 0.4405 0.053 Uiso 1 1 calc R . . C36 C 0.6384(5) -0.0996(5) 0.3746(3) 0.0363(15) Uani 1 1 d . . . H36A H 0.5759 -0.0319 0.3909 0.044 Uiso 1 1 calc R . . C37 C 0.7448(6) -0.4239(5) 0.4152(3) 0.060(2) Uani 1 1 d . . . H37A H 0.7104 -0.4188 0.4605 0.072 Uiso 1 1 calc R . . H37B H 0.8307 -0.4804 0.4119 0.072 Uiso 1 1 calc R . . C41 C 0.6562(5) 0.1962(5) 0.4627(2) 0.0272(13) Uani 1 1 d . . . C42 C 0.6807(5) 0.0866(5) 0.4943(3) 0.0409(16) Uani 1 1 d . . . H42A H 0.6977 0.0269 0.4714 0.049 Uiso 1 1 calc R . . C43 C 0.6810(6) 0.0615(6) 0.5594(3) 0.0503(18) Uani 1 1 d . . . H43A H 0.7000 -0.0149 0.5801 0.060 Uiso 1 1 calc R . . C44 C 0.6539(6) 0.1475(6) 0.5933(3) 0.0453(17) Uani 1 1 d . . . C45 C 0.6273(6) 0.2565(6) 0.5627(3) 0.056(2) Uani 1 1 d . . . H45A H 0.6085 0.3164 0.5860 0.067 Uiso 1 1 calc R . . C46 C 0.6272(6) 0.2810(5) 0.4989(3) 0.0457(17) Uani 1 1 d . . . H46A H 0.6069 0.3580 0.4790 0.055 Uiso 1 1 calc R . . C47 C 0.6573(8) 0.1246(7) 0.6645(3) 0.084(3) Uani 1 1 d . . . H47A H 0.5937 0.1931 0.6839 0.101 Uiso 1 1 calc R . . H47B H 0.7357 0.1152 0.6701 0.101 Uiso 1 1 calc R . . C51 C 0.7106(6) 0.6143(5) 0.1778(4) 0.013(3) Uiso 0.486(3) 1 d PGDU A 1 C52 C 0.6613(8) 0.6965(6) 0.2187(3) 0.025(3) Uiso 0.486(3) 1 d PGDU A 1 H52B H 0.6372 0.6763 0.2623 0.030 Uiso 0.486(3) 1 calc PR A 1 C53 C 0.6472(9) 0.8082(5) 0.1958(4) 0.032(3) Uiso 0.486(3) 1 d PGDU A 1 H53B H 0.6135 0.8644 0.2238 0.038 Uiso 0.486(3) 1 calc PR A 1 C54 C 0.6824(9) 0.8378(5) 0.1320(4) 0.034(3) Uiso 0.486(3) 1 d PGDU A 1 C55 C 0.7318(11) 0.7556(7) 0.0910(4) 0.031(3) Uiso 0.486(3) 1 d PGDU A 1 H55B H 0.7559 0.7758 0.0474 0.037 Uiso 0.486(3) 1 calc PR A 1 C56 C 0.7459(9) 0.6439(6) 0.1139(4) 0.023(3) Uiso 0.486(3) 1 d PGDU A 1 H56B H 0.7796 0.5877 0.0859 0.028 Uiso 0.486(3) 1 calc PR A 1 C57 C 0.6669(13) 0.9589(9) 0.1122(6) 0.076(5) Uiso 0.486(3) 1 d PDU A 1 H57A H 0.7161 0.9712 0.1350 0.091 Uiso 0.486(3) 1 calc PR A 1 H57B H 0.5817 1.0114 0.1261 0.091 Uiso 0.486(3) 1 calc PR A 1 C51' C 0.6919(8) 0.6214(7) 0.1782(6) 0.037(5) Uiso 0.312(5) 1 d PGDU A 2 C52' C 0.6368(14) 0.7053(9) 0.2184(6) 0.045(5) Uiso 0.312(5) 1 d PGDU A 2 H52A H 0.6135 0.6852 0.2622 0.054 Uiso 0.312(5) 1 calc PR A 2 C53' C 0.6157(15) 0.8186(8) 0.1946(7) 0.038(5) Uiso 0.312(5) 1 d PGDU A 2 H53A H 0.5780 0.8760 0.2220 0.046 Uiso 0.312(5) 1 calc PR A 2 C54' C 0.6497(10) 0.8480(7) 0.1306(7) 0.022(4) Uiso 0.312(5) 1 d PGDU A 2 C55' C 0.7048(14) 0.7641(9) 0.0904(6) 0.027(5) Uiso 0.312(5) 1 d PGDU A 2 H55A H 0.7281 0.7842 0.0467 0.033 Uiso 0.312(5) 1 calc PR A 2 C56' C 0.7259(13) 0.6508(8) 0.1142(6) 0.031(5) Uiso 0.312(5) 1 d PGDU A 2 H56A H 0.7636 0.5935 0.0868 0.037 Uiso 0.312(5) 1 calc PR A 2 C57' C 0.6233(12) 0.9711(10) 0.1052(8) 0.021(4) Uiso 0.312(5) 1 d PDU A 2 H57C H 0.5582 1.0205 0.1356 0.025 Uiso 0.312(5) 1 calc PR A 2 H57D H 0.5920 0.9906 0.0654 0.025 Uiso 0.312(5) 1 calc PR A 2 C51" C 0.7053(10) 0.6143(8) 0.1695(6) 0.028(6) Uiso 0.202(5) 1 d PGDU A -3 C52" C 0.6461(16) 0.7080(10) 0.2032(6) 0.028(5) Uiso 0.202(5) 1 d PGDU A -3 H52C H 0.6135 0.6979 0.2467 0.033 Uiso 0.202(5) 1 calc PR A -3 C53" C 0.6346(18) 0.8163(9) 0.1733(7) 0.015(5) Uiso 0.202(5) 1 d PGDU A -3 H53C H 0.5942 0.8803 0.1963 0.018 Uiso 0.202(5) 1 calc PR A -3 C54" C 0.6824(16) 0.8310(9) 0.1097(7) 0.003(4) Uiso 0.202(5) 1 d PGDU A -3 C55" C 0.742(2) 0.7374(12) 0.0761(6) 0.034(6) Uiso 0.202(5) 1 d PGDU A -3 H55C H 0.7743 0.7474 0.0326 0.041 Uiso 0.202(5) 1 calc PR A -3 C56" C 0.7531(18) 0.6291(10) 0.1060(6) 0.037(6) Uiso 0.202(5) 1 d PGDU A -3 H56C H 0.7936 0.5651 0.0830 0.045 Uiso 0.202(5) 1 calc PR A -3 C57" C 0.668(2) 0.9494(13) 0.0780(10) 0.037(6) Uiso 0.202(5) 1 d PDU A -3 H57E H 0.7484 0.9469 0.0596 0.044 Uiso 0.202(5) 1 calc PR A -3 H57F H 0.6285 1.0041 0.1095 0.044 Uiso 0.202(5) 1 calc PR A -3 C61 C 0.8180(5) 0.3094(5) 0.0371(3) 0.0288(14) Uani 1 1 d . A . C62 C 0.7554(6) 0.4080(5) -0.0018(3) 0.0450(17) Uani 1 1 d . . . H62A H 0.6767 0.4607 0.0147 0.054 Uiso 1 1 calc R A . C63 C 0.8041(6) 0.4319(6) -0.0642(3) 0.0520(18) Uani 1 1 d . A . H63A H 0.7587 0.4993 -0.0900 0.062 Uiso 1 1 calc R . . C64 C 0.9195(6) 0.3564(6) -0.0885(3) 0.0450(17) Uani 1 1 d . . . C65 C 0.9805(6) 0.2557(6) -0.0518(3) 0.0469(17) Uani 1 1 d . A . H65A H 1.0578 0.2017 -0.0691 0.056 Uiso 1 1 calc R . . C66 C 0.9307(5) 0.2320(5) 0.0102(3) 0.0370(15) Uani 1 1 d . . . H66A H 0.9742 0.1616 0.0348 0.044 Uiso 1 1 calc R A . C67 C 0.9769(7) 0.3883(7) -0.1547(3) 0.068(2) Uani 1 1 d . A . H67A H 1.0617 0.3300 -0.1631 0.081 Uiso 1 1 calc R . . H67B H 0.9769 0.4637 -0.1573 0.081 Uiso 1 1 calc R . . C71 C 1.0833(5) -0.0132(5) 0.1778(2) 0.0283(14) Uani 1 1 d . A . C72 C 1.0924(5) -0.0811(5) 0.1353(3) 0.0398(15) Uani 1 1 d . . . H72A H 1.0206 -0.0739 0.1259 0.048 Uiso 1 1 calc R A . C73 C 1.2008(6) -0.1573(5) 0.1068(3) 0.0484(17) Uani 1 1 d . A . H73A H 1.2030 -0.2017 0.0782 0.058 Uiso 1 1 calc R . . C74 C 1.3068(5) -0.1701(5) 0.1191(3) 0.0421(16) Uani 1 1 d . . . C75 C 1.3012(5) -0.1053(6) 0.1609(3) 0.0486(17) Uani 1 1 d . A . H75A H 1.3735 -0.1128 0.1696 0.058 Uiso 1 1 calc R . . C76 C 1.1912(5) -0.0292(5) 0.1906(2) 0.0355(15) Uani 1 1 d . . . H76A H 1.1897 0.0130 0.2203 0.043 Uiso 1 1 calc R A . C77 C 1.4281(6) -0.2506(6) 0.0852(3) 0.070(2) Uani 1 1 d . A . H77A H 1.4927 -0.2413 0.0964 0.084 Uiso 1 1 calc R . . H77B H 1.4307 -0.2282 0.0391 0.084 Uiso 1 1 calc R . . C81 C 0.9870(5) 0.2837(7) 0.3373(4) 0.025(3) Uani 0.595(4) 1 d PGDU A 1 C82 C 1.0315(12) 0.3654(11) 0.3166(5) 0.036(3) Uani 0.595(4) 1 d PGDU A 1 H82A H 1.0136 0.4158 0.2784 0.043 Uiso 0.595(4) 1 calc PR A 1 C83 C 1.1021(13) 0.3734(11) 0.3518(6) 0.041(3) Uani 0.595(4) 1 d PGDU A 1 H83A H 1.1325 0.4293 0.3377 0.049 Uiso 0.595(4) 1 calc PR A 1 C84 C 1.1281(7) 0.2997(9) 0.4077(5) 0.035(3) Uani 0.595(4) 1 d PGDU A 1 C85 C 1.0836(10) 0.2180(10) 0.4284(4) 0.034(3) Uani 0.595(4) 1 d PGDU A 1 H85A H 1.1015 0.1676 0.4665 0.041 Uiso 0.595(4) 1 calc PR A 1 C86 C 1.0130(10) 0.2099(9) 0.3931(4) 0.026(3) Uani 0.595(4) 1 d PGDU A 1 H86A H 0.9826 0.1541 0.4073 0.031 Uiso 0.595(4) 1 calc PR A 1 C87 C 1.2071(10) 0.3041(12) 0.4459(6) 0.057(3) Uani 0.595(4) 1 d PDU A 1 H87A H 1.1860 0.2757 0.4906 0.069 Uiso 0.595(4) 1 calc PR A 1 H87B H 1.1925 0.3850 0.4433 0.069 Uiso 0.595(4) 1 calc PR A 1 C81' C 0.9765(8) 0.2918(10) 0.3410(5) 0.031(4) Uiso 0.405(4) 1 d PGDU A -2 C82' C 1.0245(19) 0.3706(17) 0.3181(7) 0.037(4) Uiso 0.405(4) 1 d PGDU A -2 H82B H 1.0123 0.4154 0.2780 0.045 Uiso 0.405(4) 1 calc PR A -2 C83' C 1.090(2) 0.3840(18) 0.3540(8) 0.049(4) Uiso 0.405(4) 1 d PGDU A -2 H83B H 1.1232 0.4379 0.3384 0.059 Uiso 0.405(4) 1 calc PR A -2 C84' C 1.1083(11) 0.3185(13) 0.4128(7) 0.035(4) Uiso 0.405(4) 1 d PGDU A -2 C85' C 1.0603(16) 0.2396(15) 0.4356(6) 0.036(5) Uiso 0.405(4) 1 d PGDU A -2 H85B H 1.0725 0.1949 0.4758 0.043 Uiso 0.405(4) 1 calc PR A -2 C86' C 0.9944(16) 0.2263(14) 0.3997(7) 0.032(4) Uiso 0.405(4) 1 d PGDU A -2 H86B H 0.9616 0.1724 0.4153 0.038 Uiso 0.405(4) 1 calc PR A -2 C87' C 1.1768(14) 0.3351(17) 0.4529(9) 0.055(5) Uiso 0.405(4) 1 d PDU A -2 H87C H 1.2350 0.3632 0.4260 0.066 Uiso 0.405(4) 1 calc PR A -2 H87D H 1.2212 0.2615 0.4786 0.066 Uiso 0.405(4) 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 Si1 0.0243(9) 0.0191(9) 0.0324(9) -0.0041(7) -0.0063(7) -0.0079(8) Si2 0.0233(9) 0.0217(9) 0.0303(9) -0.0026(7) -0.0077(7) -0.0094(8) Si3 0.0233(9) 0.0179(9) 0.0344(10) -0.0017(7) -0.0064(7) -0.0084(8) Si4 0.0238(9) 0.0201(9) 0.0298(9) -0.0004(7) -0.0069(7) -0.0092(8) Si5 0.0269(9) 0.0185(9) 0.0291(9) -0.0012(7) -0.0071(7) -0.0100(8) Si6 0.0240(9) 0.0198(9) 0.0290(9) -0.0001(7) -0.0092(7) -0.0081(8) Si7 0.0231(9) 0.0196(9) 0.0307(9) -0.0012(7) -0.0068(7) -0.0081(8) Si8 0.0235(9) 0.0212(9) 0.0292(9) -0.0006(7) -0.0088(7) -0.0100(8) Cl1 0.0699(14) 0.0418(12) 0.1313(18) -0.0385(12) 0.0161(13) -0.0151(11) Cl2 0.0551(12) 0.0540(12) 0.1045(15) -0.0047(11) -0.0470(11) -0.0153(10) Cl3 0.1094(17) 0.0510(12) 0.0763(13) -0.0098(10) -0.0008(12) -0.0552(13) Cl4 0.0975(17) 0.1111(18) 0.0404(10) 0.0098(11) -0.0199(10) -0.0603(15) Cl5 0.126(5) 0.034(2) 0.103(4) 0.020(3) 0.041(4) -0.012(3) Cl5' 0.088(5) 0.038(4) 0.150(7) -0.015(4) 0.039(5) -0.039(3) Cl5" 0.153(9) 0.037(6) 0.089(7) 0.007(5) 0.002(7) -0.012(6) Cl6 0.0777(14) 0.0809(14) 0.0393(10) -0.0004(9) -0.0060(9) -0.0431(12) Cl7 0.0474(12) 0.0595(14) 0.1034(15) -0.0360(12) -0.0077(11) 0.0086(10) Cl8 0.043(2) 0.073(2) 0.099(3) -0.0035(19) -0.0299(17) -0.0275(18) Cl8' 0.083(4) 0.085(4) 0.058(3) -0.025(3) -0.012(3) -0.052(3) O1 0.026(2) 0.022(2) 0.041(2) -0.0040(18) -0.0123(18) -0.0060(19) O2 0.030(2) 0.019(2) 0.035(2) -0.0008(17) -0.0122(18) -0.0081(19) O3 0.028(2) 0.022(2) 0.033(2) -0.0012(17) -0.0070(17) -0.0109(18) O4 0.024(2) 0.022(2) 0.032(2) -0.0017(17) -0.0099(17) -0.0040(18) O5 0.027(2) 0.021(2) 0.033(2) -0.0026(17) -0.0070(17) -0.0084(18) O6 0.029(2) 0.032(2) 0.038(2) 0.0017(18) -0.0112(18) -0.018(2) O7 0.026(2) 0.025(2) 0.037(2) 0.0018(18) -0.0116(18) -0.0091(19) O8 0.026(2) 0.026(2) 0.039(2) 0.0010(18) -0.0132(18) -0.0112(19) O9 0.027(2) 0.020(2) 0.035(2) 0.0008(17) -0.0078(17) -0.0084(18) O10 0.029(2) 0.019(2) 0.036(2) 0.0026(17) -0.0114(18) -0.0064(19) O11 0.027(2) 0.028(2) 0.035(2) -0.0085(18) -0.0050(17) -0.0109(19) O12 0.029(2) 0.026(2) 0.033(2) 0.0040(17) -0.0113(18) -0.0124(19) C11 0.034(4) 0.020(3) 0.030(3) -0.001(3) -0.013(3) -0.015(3) C12 0.035(4) 0.024(4) 0.038(4) 0.001(3) -0.011(3) -0.002(3) C13 0.041(4) 0.038(4) 0.042(4) -0.010(3) 0.004(3) -0.010(4) C14 0.028(4) 0.032(4) 0.051(4) -0.013(3) -0.003(3) -0.010(3) C15 0.047(4) 0.029(4) 0.049(4) 0.002(3) -0.016(4) 0.001(3) C16 0.043(4) 0.033(4) 0.034(4) -0.004(3) -0.008(3) -0.003(3) C17 0.035(4) 0.037(4) 0.084(5) -0.014(4) -0.011(4) 0.002(4) C21 0.020(3) 0.020(3) 0.034(3) -0.005(3) -0.004(3) -0.008(3) C22 0.044(4) 0.068(5) 0.027(3) -0.006(3) -0.007(3) -0.037(4) C23 0.044(4) 0.076(5) 0.037(4) -0.013(4) 0.006(3) -0.043(4) C24 0.032(4) 0.027(4) 0.048(4) -0.003(3) -0.013(3) -0.012(3) C25 0.043(4) 0.058(4) 0.029(3) -0.004(3) -0.012(3) -0.027(4) C26 0.027(4) 0.044(4) 0.033(4) -0.006(3) -0.005(3) -0.019(3) C27 0.041(4) 0.052(4) 0.050(4) -0.001(3) -0.015(3) -0.028(4) C31 0.025(3) 0.027(3) 0.031(3) -0.003(3) -0.010(3) -0.011(3) C32 0.047(4) 0.028(4) 0.040(4) -0.004(3) 0.003(3) -0.016(3) C33 0.059(5) 0.019(4) 0.058(4) -0.011(3) 0.008(4) -0.010(3) C34 0.044(4) 0.026(4) 0.052(4) 0.002(3) -0.008(3) -0.019(4) C35 0.038(4) 0.041(4) 0.053(4) -0.002(3) 0.003(3) -0.024(4) C36 0.028(4) 0.027(4) 0.050(4) -0.008(3) 0.005(3) -0.013(3) C37 0.063(5) 0.038(4) 0.078(5) -0.007(4) -0.007(4) -0.023(4) C41 0.020(3) 0.029(4) 0.033(3) -0.005(3) -0.008(3) -0.010(3) C42 0.048(4) 0.036(4) 0.031(4) -0.004(3) -0.008(3) -0.012(3) C43 0.057(5) 0.039(4) 0.035(4) 0.013(3) -0.015(3) -0.010(4) C44 0.052(4) 0.058(5) 0.034(4) -0.002(4) -0.014(3) -0.029(4) C45 0.078(5) 0.065(5) 0.048(5) -0.023(4) 0.004(4) -0.050(5) C46 0.072(5) 0.040(4) 0.036(4) -0.003(3) -0.006(3) -0.035(4) C47 0.108(7) 0.115(7) 0.054(5) -0.013(5) -0.010(5) -0.070(6) C61 0.029(4) 0.020(3) 0.042(4) -0.005(3) -0.015(3) -0.010(3) C62 0.047(4) 0.033(4) 0.038(4) -0.009(3) -0.001(3) -0.005(3) C63 0.069(5) 0.036(4) 0.036(4) 0.005(3) -0.005(4) -0.018(4) C64 0.058(5) 0.055(5) 0.033(4) -0.014(4) 0.005(4) -0.036(4) C65 0.034(4) 0.051(5) 0.051(4) -0.017(4) 0.001(3) -0.014(4) C66 0.040(4) 0.036(4) 0.035(4) -0.004(3) -0.009(3) -0.016(3) C67 0.082(6) 0.087(6) 0.048(4) -0.014(4) -0.003(4) -0.049(5) C71 0.034(4) 0.030(4) 0.025(3) 0.004(3) -0.010(3) -0.018(3) C72 0.024(4) 0.038(4) 0.056(4) -0.016(3) -0.007(3) -0.008(3) C73 0.040(4) 0.043(4) 0.059(4) -0.027(4) 0.001(3) -0.011(4) C74 0.021(4) 0.044(4) 0.050(4) -0.012(3) 0.001(3) -0.006(3) C75 0.025(4) 0.066(5) 0.051(4) -0.004(4) -0.012(3) -0.015(4) C76 0.031(4) 0.040(4) 0.037(4) -0.012(3) -0.007(3) -0.013(3) C77 0.029(4) 0.069(5) 0.080(5) -0.013(4) 0.007(4) -0.002(4) C81 0.019(5) 0.020(5) 0.036(5) -0.008(4) 0.000(4) -0.010(4) C82 0.034(5) 0.032(5) 0.043(6) 0.000(4) -0.010(4) -0.016(5) C83 0.039(6) 0.044(6) 0.057(6) -0.008(5) -0.012(5) -0.030(5) C84 0.028(5) 0.036(6) 0.051(6) -0.025(5) -0.012(5) -0.010(5) C85 0.028(6) 0.037(6) 0.035(5) -0.005(5) -0.012(5) -0.009(6) C86 0.025(5) 0.020(5) 0.035(5) -0.004(4) -0.008(5) -0.009(5) C87 0.056(7) 0.077(8) 0.055(6) -0.006(6) -0.033(6) -0.031(7) _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 O5 1.610(3) . ? Si1 O4 1.617(3) . ? Si1 O1 1.618(3) . ? Si1 C11 1.833(6) . ? Si2 O1 1.612(3) . ? Si2 O6 1.619(4) . ? Si2 O2 1.627(4) . ? Si2 C21 1.854(5) . ? Si3 O3 1.615(3) . ? Si3 O2 1.619(4) . ? Si3 O7 1.620(4) . ? Si3 C31 1.847(5) . ? Si4 O8 1.602(3) . ? Si4 O3 1.619(3) . ? Si4 O4 1.626(4) . ? Si4 C41 1.829(5) . ? Si5 O9 1.611(3) . ? Si5 O5 1.618(3) . ? Si5 O12 1.622(4) . ? Si5 C51 1.854(5) . ? Si5 C51" 1.868(8) . ? Si5 C51' 1.870(7) . ? Si6 O9 1.616(3) . ? Si6 O6 1.618(3) . ? Si6 O10 1.618(4) . ? Si6 C61 1.831(6) . ? Si7 O10 1.607(3) . ? Si7 O7 1.624(4) . ? Si7 O11 1.625(3) . ? Si7 C71 1.832(6) . ? Si8 O8 1.612(4) . ? Si8 O12 1.613(4) . ? Si8 O11 1.626(3) . ? Si8 C81 1.860(5) . ? Si8 C81' 1.865(7) . ? Cl1 C17 1.751(6) . ? Cl2 C27 1.773(6) . ? Cl3 C37 1.761(6) . ? Cl4 C47 1.724(7) . ? Cl5 C57 1.741(12) . ? Cl5' C57' 1.783(12) . ? Cl5" C57" 1.780(16) . ? Cl6 C67 1.752(6) . ? Cl7 C77 1.758(7) . ? Cl8 C87 1.765(12) . ? Cl8' C87' 1.828(15) . ? C11 C12 1.390(7) . ? C11 C16 1.391(7) . ? C12 C13 1.383(7) . ? C13 C14 1.388(8) . ? C14 C15 1.365(7) . ? C14 C17 1.505(7) . ? C15 C16 1.403(8) . ? C21 C22 1.365(7) . ? C21 C26 1.392(7) . ? C22 C23 1.390(7) . ? C23 C24 1.363(7) . ? C24 C25 1.383(7) . ? C24 C27 1.518(7) . ? C25 C26 1.388(7) . ? C31 C36 1.383(7) . ? C31 C32 1.397(7) . ? C32 C33 1.382(7) . ? C33 C34 1.397(8) . ? C34 C35 1.381(7) . ? C34 C37 1.513(8) . ? C35 C36 1.392(7) . ? C41 C42 1.382(7) . ? C41 C46 1.390(7) . ? C42 C43 1.401(7) . ? C43 C44 1.373(8) . ? C44 C45 1.364(8) . ? C44 C47 1.540(8) . ? C45 C46 1.373(8) . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C54 C57 1.493(9) . ? C55 C56 1.3900 . ? C51' C52' 1.3900 . ? C51' C56' 1.3900 . ? C52' C53' 1.3900 . ? C53' C54' 1.3900 . ? C54' C55' 1.3900 . ? C54' C57' 1.497(9) . ? C55' C56' 1.3900 . ? C51" C52" 1.3900 . ? C51" C56" 1.3900 . ? C52" C53" 1.3900 . ? C53" C54" 1.3900 . ? C54" C55" 1.3900 . ? C54" C57" 1.508(10) . ? C55" C56" 1.3900 . ? C61 C62 1.388(7) . ? C61 C66 1.391(7) . ? C62 C63 1.392(7) . ? C63 C64 1.385(8) . ? C64 C65 1.372(8) . ? C64 C67 1.521(8) . ? C65 C66 1.389(7) . ? C71 C76 1.390(7) . ? C71 C72 1.401(7) . ? C72 C73 1.367(7) . ? C73 C74 1.378(8) . ? C74 C75 1.373(8) . ? C74 C77 1.525(8) . ? C75 C76 1.387(8) . ? C81 C82 1.3900 . ? C81 C86 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? C84 C87 1.504(7) . ? C85 C86 1.3900 . ? C81' C82' 1.3900 . ? C81' C86' 1.3900 . ? C82' C83' 1.3900 . ? C83' C84' 1.3900 . ? C84' C85' 1.3900 . ? C84' C87' 1.513(10) . ? C85' C86' 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Si1 O4 109.98(18) . . ? O5 Si1 O1 107.93(18) . . ? O4 Si1 O1 109.51(18) . . ? O5 Si1 C11 110.8(2) . . ? O4 Si1 C11 105.7(2) . . ? O1 Si1 C11 112.9(2) . . ? O1 Si2 O6 110.68(18) . . ? O1 Si2 O2 108.60(18) . . ? O6 Si2 O2 108.80(19) . . ? O1 Si2 C21 110.7(2) . . ? O6 Si2 C21 107.2(2) . . ? O2 Si2 C21 110.9(2) . . ? O3 Si3 O2 108.55(18) . . ? O3 Si3 O7 109.97(18) . . ? O2 Si3 O7 109.42(18) . . ? O3 Si3 C31 105.8(2) . . ? O2 Si3 C31 113.4(2) . . ? O7 Si3 C31 109.5(2) . . ? O8 Si4 O3 108.29(18) . . ? O8 Si4 O4 107.35(18) . . ? O3 Si4 O4 108.98(18) . . ? O8 Si4 C41 111.0(2) . . ? O3 Si4 C41 109.9(2) . . ? O4 Si4 C41 111.2(2) . . ? O9 Si5 O5 110.22(18) . . ? O9 Si5 O12 108.14(18) . . ? O5 Si5 O12 108.56(18) . . ? O9 Si5 C51 108.8(3) . . ? O5 Si5 C51 110.4(3) . . ? O12 Si5 C51 110.7(2) . . ? O9 Si5 C51" 103.0(4) . . ? O5 Si5 C51" 110.9(4) . . ? O12 Si5 C51" 115.9(3) . . ? O9 Si5 C51' 108.8(4) . . ? O5 Si5 C51' 104.8(4) . . ? O12 Si5 C51' 116.2(3) . . ? O9 Si6 O6 107.64(19) . . ? O9 Si6 O10 109.44(18) . . ? O6 Si6 O10 109.01(18) . . ? O9 Si6 C61 108.4(2) . . ? O6 Si6 C61 113.8(2) . . ? O10 Si6 C61 108.6(2) . . ? O10 Si7 O7 107.37(18) . . ? O10 Si7 O11 109.78(18) . . ? O7 Si7 O11 110.73(18) . . ? O10 Si7 C71 108.0(2) . . ? O7 Si7 C71 112.3(2) . . ? O11 Si7 C71 108.6(2) . . ? O8 Si8 O12 111.40(18) . . ? O8 Si8 O11 106.96(18) . . ? O12 Si8 O11 108.50(18) . . ? O8 Si8 C81 109.0(3) . . ? O12 Si8 C81 109.4(3) . . ? O11 Si8 C81 111.6(2) . . ? O8 Si8 C81' 106.2(4) . . ? O12 Si8 C81' 107.8(4) . . ? O11 Si8 C81' 115.9(3) . . ? Si2 O1 Si1 155.3(2) . . ? Si3 O2 Si2 147.6(2) . . ? Si3 O3 Si4 146.3(2) . . ? Si1 O4 Si4 138.8(2) . . ? Si1 O5 Si5 152.5(2) . . ? Si6 O6 Si2 142.1(2) . . ? Si3 O7 Si7 147.9(2) . . ? Si4 O8 Si8 164.2(2) . . ? Si5 O9 Si6 150.6(2) . . ? Si7 O10 Si6 154.9(2) . . ? Si7 O11 Si8 141.2(2) . . ? Si8 O12 Si5 142.9(2) . . ? C12 C11 C16 116.7(5) . . ? C12 C11 Si1 121.7(4) . . ? C16 C11 Si1 121.6(4) . . ? C13 C12 C11 121.9(5) . . ? C12 C13 C14 120.9(5) . . ? C15 C14 C13 118.0(6) . . ? C15 C14 C17 121.1(6) . . ? C13 C14 C17 120.9(6) . . ? C14 C15 C16 121.3(6) . . ? C11 C16 C15 121.1(5) . . ? C14 C17 Cl1 112.6(4) . . ? C22 C21 C26 117.6(5) . . ? C22 C21 Si2 122.0(4) . . ? C26 C21 Si2 120.4(4) . . ? C21 C22 C23 121.7(5) . . ? C24 C23 C22 120.8(5) . . ? C23 C24 C25 118.3(5) . . ? C23 C24 C27 120.3(5) . . ? C25 C24 C27 121.3(5) . . ? C24 C25 C26 121.0(5) . . ? C25 C26 C21 120.5(5) . . ? C24 C27 Cl2 111.2(4) . . ? C36 C31 C32 117.9(5) . . ? C36 C31 Si3 119.5(4) . . ? C32 C31 Si3 122.3(4) . . ? C33 C32 C31 120.6(5) . . ? C32 C33 C34 121.4(5) . . ? C35 C34 C33 117.7(5) . . ? C35 C34 C37 121.0(5) . . ? C33 C34 C37 121.3(6) . . ? C34 C35 C36 120.9(5) . . ? C31 C36 C35 121.3(5) . . ? C34 C37 Cl3 111.2(5) . . ? C42 C41 C46 116.8(5) . . ? C42 C41 Si4 121.9(4) . . ? C46 C41 Si4 121.3(4) . . ? C41 C42 C43 121.5(5) . . ? C44 C43 C42 119.9(6) . . ? C45 C44 C43 119.2(6) . . ? C45 C44 C47 118.4(6) . . ? C43 C44 C47 122.3(6) . . ? C44 C45 C46 121.0(6) . . ? C45 C46 C41 121.7(6) . . ? C44 C47 Cl4 114.9(5) . . ? C52 C51 C56 120.0 . . ? C52 C51 Si5 119.1(4) . . ? C56 C51 Si5 120.8(4) . . ? C53 C52 C51 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? C53 C54 C57 116.1(6) . . ? C55 C54 C57 123.9(6) . . ? C56 C55 C54 120.0 . . ? C55 C56 C51 120.0 . . ? C54 C57 Cl5 116.6(8) . . ? C52' C51' C56' 120.0 . . ? C52' C51' Si5 121.1(6) . . ? C56' C51' Si5 118.9(6) . . ? C53' C52' C51' 120.0 . . ? C52' C53' C54' 120.0 . . ? C55' C54' C53' 120.0 . . ? C55' C54' C57' 120.5(7) . . ? C53' C54' C57' 119.4(7) . . ? C56' C55' C54' 120.0 . . ? C55' C56' C51' 120.0 . . ? C54' C57' Cl5' 116.4(7) . . ? C52" C51" C56" 120.0 . . ? C52" C51" Si5 120.5(6) . . ? C56" C51" Si5 119.4(6) . . ? C53" C52" C51" 120.0 . . ? C52" C53" C54" 120.0 . . ? C53" C54" C55" 120.0 . . ? C53" C54" C57" 119.2(7) . . ? C55" C54" C57" 120.8(7) . . ? C54" C55" C56" 120.0 . . ? C55" C56" C51" 120.0 . . ? C54" C57" Cl5" 109.8(8) . . ? C62 C61 C66 117.1(5) . . ? C62 C61 Si6 121.6(4) . . ? C66 C61 Si6 120.7(4) . . ? C61 C62 C63 122.1(6) . . ? C64 C63 C62 119.4(6) . . ? C65 C64 C63 119.3(6) . . ? C65 C64 C67 121.4(6) . . ? C63 C64 C67 119.2(7) . . ? C64 C65 C66 120.8(6) . . ? C65 C66 C61 121.1(6) . . ? C64 C67 Cl6 112.1(5) . . ? C76 C71 C72 116.2(5) . . ? C76 C71 Si7 122.5(4) . . ? C72 C71 Si7 121.2(4) . . ? C73 C72 C71 122.3(5) . . ? C72 C73 C74 120.6(6) . . ? C75 C74 C73 118.6(5) . . ? C75 C74 C77 120.4(6) . . ? C73 C74 C77 120.9(6) . . ? C74 C75 C76 120.9(5) . . ? C75 C76 C71 121.4(5) . . ? C74 C77 Cl7 112.8(5) . . ? C82 C81 C86 120.0 . . ? C82 C81 Si8 121.7(4) . . ? C86 C81 Si8 118.3(4) . . ? C83 C82 C81 120.0 . . ? C84 C83 C82 120.0 . . ? C85 C84 C83 120.0 . . ? C85 C84 C87 118.8(6) . . ? C83 C84 C87 121.2(6) . . ? C84 C85 C86 120.0 . . ? C85 C86 C81 120.0 . . ? C84 C87 Cl8 111.4(6) . . ? C82' C81' C86' 120.0 . . ? C82' C81' Si8 120.6(6) . . ? C86' C81' Si8 119.4(6) . . ? C81' C82' C83' 120.0 . . ? C84' C83' C82' 120.0 . . ? C83' C84' C85' 120.0 . . ? C83' C84' C87' 120.2(7) . . ? C85' C84' C87' 119.7(7) . . ? C86' C85' C84' 120.0 . . ? C85' C86' C81' 120.0 . . ? C84' C87' Cl8' 106.1(7) . . ? _diffrn_measured_fraction_theta_max 0.794 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.445 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.077 #===END