# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Jihua Chen' 'John E. Anthony' 'Kaitlin Gallup' 'Chelsea Haughn' 'David C. Martin' 'Sean Parkin' 'Maxime Siegler' 'Sankar Subramanian' _publ_contact_author_name 'Jihua Chen' _publ_contact_author_address ; Chemical Engineering and Materials Science University of Minnesota at Twin Cities 1420 Terrace Dr. Apt 306 Roseville MN 55113 UNITED STATES OF AMERICA ; _publ_contact_author_email CHENX486@UMN.EDU _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; The Influence of Side Chains on the Structures and Properties of Functionalized Pentacenes ; data_k04106 _database_code_depnum_ccdc_archive 'CCDC 671507' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H30' _chemical_formula_sum 'C34 H30' _chemical_formula_weight 438.58 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 19.8513(4) _cell_length_b 5.30060(10) _cell_length_c 22.6989(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.5526(8) _cell_angle_gamma 90.00 _cell_volume 2383.87(8) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 4886 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.35 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour black _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9632 _exptl_absorpt_correction_T_max 0.9898 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\w scans at fixed \c = 55\%' _diffrn_detector_area_resol_mean 18 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 7929 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0813 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4214 _reflns_number_gt 2358 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material ; SHELX97-2 (Sheldrick, 1997) and local procedures ; _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^)+(0.0550P)^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 4214 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1163 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.54933(10) 0.4389(4) -0.04073(8) 0.0198(5) Uani 1 1 d . . . C2 C 0.48839(10) 0.2985(4) -0.04113(8) 0.0191(5) Uani 1 1 d . . . C3 C 0.47505(10) 0.0991(4) -0.08093(8) 0.0214(5) Uani 1 1 d . . . H3 H 0.5079 0.0578 -0.1081 0.026 Uiso 1 1 calc R . . C4 C 0.41586(10) -0.0394(4) -0.08199(8) 0.0205(5) Uani 1 1 d . . . C5 C 0.40221(10) -0.2422(4) -0.12240(8) 0.0248(5) Uani 1 1 d . . . H5 H 0.4342 -0.2820 -0.1505 0.030 Uiso 1 1 calc R . . C6 C 0.34457(10) -0.3791(4) -0.12157(8) 0.0259(5) Uani 1 1 d . . . H6 H 0.3366 -0.5136 -0.1488 0.031 Uiso 1 1 calc R . . C7 C 0.29592(10) -0.3217(4) -0.07995(9) 0.0257(5) Uani 1 1 d . . . H7 H 0.2557 -0.4187 -0.0795 0.031 Uiso 1 1 calc R . . C8 C 0.30644(10) -0.1301(4) -0.04104(9) 0.0241(5) Uani 1 1 d . . . H8 H 0.2734 -0.0945 -0.0137 0.029 Uiso 1 1 calc R . . C9 C 0.36644(10) 0.0200(4) -0.04033(8) 0.0203(5) Uani 1 1 d . . . C10 C 0.37913(10) 0.2152(4) -0.00074(8) 0.0209(5) Uani 1 1 d . . . H10 H 0.3464 0.2534 0.0267 0.025 Uiso 1 1 calc R . . C11 C 0.43870(10) 0.3593(4) 0.00033(8) 0.0193(5) Uani 1 1 d . . . C12 C 0.59943(10) 0.3699(4) -0.08028(8) 0.0225(5) Uani 1 1 d . . . C13 C 0.64079(10) 0.2970(4) -0.11254(9) 0.0238(5) Uani 1 1 d . . . C14 C 0.69036(10) 0.1920(4) -0.15136(9) 0.0301(6) Uani 1 1 d . . . H14A H 0.7336 0.1638 -0.1282 0.036 Uiso 1 1 calc R . . H14B H 0.6986 0.3154 -0.1828 0.036 Uiso 1 1 calc R . . C15 C 0.66633(11) -0.0583(4) -0.17975(9) 0.0343(6) Uani 1 1 d . . . H15A H 0.7033 -0.1308 -0.2017 0.041 Uiso 1 1 calc R . . H15B H 0.6561 -0.1788 -0.1482 0.041 Uiso 1 1 calc R . . C16 C 0.60507(11) -0.0292(4) -0.22101(9) 0.0377(6) Uani 1 1 d . . . H16A H 0.6153 0.0906 -0.2527 0.045 Uiso 1 1 calc R . . H16B H 0.5681 0.0441 -0.1991 0.045 Uiso 1 1 calc R . . C17 C 0.58094(11) -0.2785(4) -0.24904(9) 0.0410(6) Uani 1 1 d . . . H17A H 0.6177 -0.3547 -0.2698 0.061 Uiso 1 1 calc R . . H17B H 0.5423 -0.2467 -0.2771 0.061 Uiso 1 1 calc R . . H17C H 0.5674 -0.3937 -0.2182 0.061 Uiso 1 1 calc R . . C18 C -0.01577(10) -0.5449(4) 0.05956(8) 0.0200(5) Uani 1 1 d . . . C19 C 0.03003(10) -0.3493(4) 0.04677(8) 0.0199(5) Uani 1 1 d . . . C20 C 0.06060(10) -0.1975(4) 0.09138(8) 0.0223(5) Uani 1 1 d . . . H20 H 0.0499 -0.2258 0.1311 0.027 Uiso 1 1 calc R . . C21 C 0.10593(10) -0.0076(4) 0.07967(9) 0.0215(5) Uani 1 1 d . . . C22 C 0.13712(10) 0.1471(4) 0.12504(9) 0.0252(5) Uani 1 1 d . . . H22 H 0.1273 0.1189 0.1649 0.030 Uiso 1 1 calc R . . C23 C 0.18037(10) 0.3329(4) 0.11218(9) 0.0267(5) Uani 1 1 d . . . H23 H 0.2004 0.4339 0.1431 0.032 Uiso 1 1 calc R . . C24 C 0.19641(10) 0.3795(4) 0.05288(9) 0.0250(5) Uani 1 1 d . . . H24 H 0.2273 0.5094 0.0445 0.030 Uiso 1 1 calc R . . C25 C 0.16751(9) 0.2382(4) 0.00833(9) 0.0243(5) Uani 1 1 d . . . H25 H 0.1781 0.2724 -0.0311 0.029 Uiso 1 1 calc R . . C26 C 0.12160(10) 0.0392(4) 0.01950(8) 0.0200(5) Uani 1 1 d . . . C27 C 0.09166(9) -0.1090(4) -0.02486(9) 0.0213(5) Uani 1 1 d . . . H27 H 0.1022 -0.0779 -0.0645 0.026 Uiso 1 1 calc R . . C28 C 0.04599(9) -0.3050(4) -0.01346(8) 0.0206(5) Uani 1 1 d . . . C29 C -0.03227(10) -0.5884(4) 0.11917(9) 0.0229(5) Uani 1 1 d . . . C30 C -0.04591(10) -0.6310(4) 0.16880(9) 0.0250(5) Uani 1 1 d . . . C31 C -0.06518(10) -0.6990(4) 0.22823(8) 0.0287(6) Uani 1 1 d . . . H31A H -0.0897 -0.5560 0.2450 0.034 Uiso 1 1 calc R . . H31B H -0.0239 -0.7295 0.2540 0.034 Uiso 1 1 calc R . . C32 C -0.10971(10) -0.9341(4) 0.22779(9) 0.0318(6) Uani 1 1 d . . . H32A H -0.0867 -1.0727 0.2078 0.038 Uiso 1 1 calc R . . H32B H -0.1153 -0.9871 0.2690 0.038 Uiso 1 1 calc R . . C33 C -0.17882(11) -0.8938(4) 0.19700(10) 0.0369(6) Uani 1 1 d . . . H33A H -0.1733 -0.8179 0.1577 0.044 Uiso 1 1 calc R . . H33B H -0.2044 -0.7731 0.2202 0.044 Uiso 1 1 calc R . . C34 C -0.21927(11) -1.1373(4) 0.18913(10) 0.0478(7) Uani 1 1 d . . . H34A H -0.1953 -1.2546 0.1644 0.072 Uiso 1 1 calc R . . H34B H -0.2638 -1.0997 0.1701 0.072 Uiso 1 1 calc R . . H34C H -0.2247 -1.2142 0.2278 0.072 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 C1 0.0203(12) 0.0209(13) 0.0184(11) 0.0026(10) 0.0016(9) 0.0020(10) C2 0.0202(12) 0.0192(12) 0.0178(11) 0.0020(10) 0.0006(9) 0.0017(10) C3 0.0246(13) 0.0205(13) 0.0194(12) 0.0028(10) 0.0029(10) 0.0050(11) C4 0.0225(13) 0.0183(13) 0.0205(11) 0.0025(10) -0.0014(10) 0.0033(11) C5 0.0288(13) 0.0235(13) 0.0224(12) -0.0003(11) 0.0038(10) -0.0008(11) C6 0.0337(14) 0.0201(13) 0.0235(12) -0.0033(10) -0.0006(11) -0.0010(12) C7 0.0252(13) 0.0230(14) 0.0283(12) 0.0026(11) -0.0022(10) -0.0048(11) C8 0.0236(13) 0.0235(13) 0.0254(12) 0.0038(11) 0.0030(10) 0.0006(11) C9 0.0235(13) 0.0185(13) 0.0188(11) 0.0044(10) -0.0004(10) 0.0016(11) C10 0.0208(12) 0.0213(13) 0.0208(11) 0.0009(10) 0.0036(9) 0.0041(10) C11 0.0207(12) 0.0179(13) 0.0190(11) 0.0022(10) -0.0014(10) 0.0018(10) C12 0.0261(13) 0.0186(13) 0.0228(12) -0.0012(10) 0.0018(10) -0.0038(11) C13 0.0261(13) 0.0190(13) 0.0266(12) -0.0037(11) 0.0031(10) -0.0047(11) C14 0.0259(13) 0.0307(15) 0.0343(13) -0.0081(11) 0.0067(11) -0.0051(11) C15 0.0349(14) 0.0355(15) 0.0336(14) -0.0062(12) 0.0099(11) 0.0051(12) C16 0.0397(15) 0.0443(16) 0.0290(13) -0.0086(12) 0.0021(12) 0.0033(13) C17 0.0413(15) 0.0417(16) 0.0394(14) -0.0115(13) -0.0020(12) -0.0072(13) C18 0.0201(12) 0.0182(12) 0.0220(12) 0.0020(10) 0.0033(10) 0.0027(10) C19 0.0204(12) 0.0204(13) 0.0192(11) 0.0010(10) 0.0024(9) 0.0036(10) C20 0.0251(13) 0.0240(14) 0.0180(11) -0.0012(10) 0.0039(10) 0.0011(11) C21 0.0206(12) 0.0200(13) 0.0240(12) 0.0012(10) 0.0024(10) 0.0022(11) C22 0.0282(13) 0.0260(14) 0.0212(12) 0.0002(11) 0.0011(10) 0.0000(11) C23 0.0273(13) 0.0260(14) 0.0262(13) -0.0061(11) -0.0030(10) -0.0028(11) C24 0.0203(12) 0.0233(13) 0.0316(13) -0.0001(11) 0.0029(10) -0.0021(11) C25 0.0237(13) 0.0242(13) 0.0255(12) 0.0007(11) 0.0054(10) -0.0027(11) C26 0.0178(12) 0.0180(13) 0.0244(12) -0.0004(10) 0.0028(10) 0.0020(10) C27 0.0230(12) 0.0213(13) 0.0200(12) 0.0021(10) 0.0030(10) 0.0013(11) C28 0.0185(12) 0.0172(13) 0.0261(12) -0.0003(10) 0.0023(10) 0.0021(10) C29 0.0240(13) 0.0194(13) 0.0255(13) -0.0026(10) 0.0016(11) -0.0019(10) C30 0.0270(13) 0.0227(13) 0.0253(13) -0.0009(11) 0.0007(11) -0.0059(11) C31 0.0328(13) 0.0329(14) 0.0204(12) 0.0015(11) 0.0025(10) -0.0052(12) C32 0.0349(14) 0.0338(15) 0.0271(13) 0.0081(11) 0.0059(11) -0.0058(12) C33 0.0328(14) 0.0374(15) 0.0410(15) 0.0075(12) 0.0065(12) -0.0002(12) C34 0.0394(15) 0.0433(17) 0.0598(17) 0.0126(14) -0.0038(13) -0.0167(14) _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 C1 C11 1.420(3) 3_665 ? C1 C2 1.420(3) . ? C1 C12 1.428(3) . ? C2 C3 1.405(3) . ? C2 C11 1.441(3) . ? C3 C4 1.385(3) . ? C3 H3 0.9500 . ? C4 C5 1.428(3) . ? C4 C9 1.439(3) . ? C5 C6 1.356(3) . ? C5 H5 0.9500 . ? C6 C7 1.425(3) . ? C6 H6 0.9500 . ? C7 C8 1.354(3) . ? C7 H7 0.9500 . ? C8 C9 1.432(3) . ? C8 H8 0.9500 . ? C9 C10 1.383(3) . ? C10 C11 1.407(3) . ? C10 H10 0.9500 . ? C11 C1 1.420(3) 3_665 ? C12 C13 1.198(3) . ? C13 C14 1.471(3) . ? C14 C15 1.538(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.496(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.531(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C28 1.418(3) 3_545 ? C18 C19 1.421(3) . ? C18 C29 1.430(3) . ? C19 C20 1.402(3) . ? C19 C28 1.442(3) . ? C20 C21 1.387(2) . ? C20 H20 0.9500 . ? C21 C22 1.427(3) . ? C21 C26 1.441(3) . ? C22 C23 1.350(2) . ? C22 H22 0.9500 . ? C23 C24 1.424(3) . ? C23 H23 0.9500 . ? C24 C25 1.357(2) . ? C24 H24 0.9500 . ? C25 C26 1.427(3) . ? C25 H25 0.9500 . ? C26 C27 1.382(3) . ? C27 C28 1.413(3) . ? C27 H27 0.9500 . ? C28 C18 1.418(3) 3_545 ? C29 C30 1.196(2) . ? C30 C31 1.470(3) . ? C31 C32 1.528(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.516(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.525(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 C1 C2 120.49(17) 3_665 . ? C11 C1 C12 120.26(18) 3_665 . ? C2 C1 C12 119.22(18) . . ? C3 C2 C1 121.66(18) . . ? C3 C2 C11 118.59(18) . . ? C1 C2 C11 119.75(17) . . ? C4 C3 C2 122.43(19) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C5 122.51(19) . . ? C3 C4 C9 119.00(19) . . ? C5 C4 C9 118.48(19) . . ? C6 C5 C4 121.37(19) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 120.13(19) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 120.6(2) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 121.25(19) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 122.74(19) . . ? C10 C9 C4 119.11(19) . . ? C8 C9 C4 118.14(18) . . ? C9 C10 C11 122.43(19) . . ? C9 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C10 C11 C1 121.81(18) . 3_665 ? C10 C11 C2 118.44(18) . . ? C1 C11 C2 119.75(17) 3_665 . ? C13 C12 C1 176.0(2) . . ? C12 C13 C14 176.6(2) . . ? C13 C14 C15 112.09(17) . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14B 109.2 . . ? C15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 113.08(18) . . ? C16 C15 H15A 109.0 . . ? C14 C15 H15A 109.0 . . ? C16 C15 H15B 109.0 . . ? C14 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C15 C16 C17 113.09(19) . . ? C15 C16 H16A 109.0 . . ? C17 C16 H16A 109.0 . . ? C15 C16 H16B 109.0 . . ? C17 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C28 C18 C19 120.37(17) 3_545 . ? C28 C18 C29 119.75(18) 3_545 . ? C19 C18 C29 119.87(18) . . ? C20 C19 C18 121.67(18) . . ? C20 C19 C28 118.74(18) . . ? C18 C19 C28 119.58(17) . . ? C21 C20 C19 122.35(18) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C20 C21 C22 122.43(18) . . ? C20 C21 C26 119.16(19) . . ? C22 C21 C26 118.40(19) . . ? C23 C22 C21 121.08(19) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 120.88(19) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 120.0(2) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 121.39(19) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C27 C26 C25 122.76(18) . . ? C27 C26 C21 118.98(18) . . ? C25 C26 C21 118.25(18) . . ? C26 C27 C28 122.42(18) . . ? C26 C27 H27 118.8 . . ? C28 C27 H27 118.8 . . ? C27 C28 C18 121.62(18) . 3_545 ? C27 C28 C19 118.34(18) . . ? C18 C28 C19 120.04(18) 3_545 . ? C30 C29 C18 178.4(2) . . ? C29 C30 C31 176.0(2) . . ? C30 C31 C32 112.17(17) . . ? C30 C31 H31A 109.2 . . ? C32 C31 H31A 109.2 . . ? C30 C31 H31B 109.2 . . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C33 C32 C31 113.26(18) . . ? C33 C32 H32A 108.9 . . ? C31 C32 H32A 108.9 . . ? C33 C32 H32B 108.9 . . ? C31 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? C32 C33 C34 112.94(18) . . ? C32 C33 H33A 109.0 . . ? C34 C33 H33A 109.0 . . ? C32 C33 H33B 109.0 . . ? C34 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C1 C2 C3 179.53(17) 3_665 . . . ? C12 C1 C2 C3 -2.3(3) . . . . ? C11 C1 C2 C11 -0.8(3) 3_665 . . . ? C12 C1 C2 C11 177.29(18) . . . . ? C1 C2 C3 C4 -179.89(18) . . . . ? C11 C2 C3 C4 0.5(3) . . . . ? C2 C3 C4 C5 180.00(17) . . . . ? C2 C3 C4 C9 -0.9(3) . . . . ? C3 C4 C5 C6 178.32(19) . . . . ? C9 C4 C5 C6 -0.8(3) . . . . ? C4 C5 C6 C7 0.2(3) . . . . ? C5 C6 C7 C8 0.2(3) . . . . ? C6 C7 C8 C9 -0.1(3) . . . . ? C7 C8 C9 C10 -179.25(18) . . . . ? C7 C8 C9 C4 -0.5(3) . . . . ? C3 C4 C9 C10 0.6(3) . . . . ? C5 C4 C9 C10 179.71(17) . . . . ? C3 C4 C9 C8 -178.25(17) . . . . ? C5 C4 C9 C8 0.9(3) . . . . ? C8 C9 C10 C11 178.94(17) . . . . ? C4 C9 C10 C11 0.2(3) . . . . ? C9 C10 C11 C1 179.20(17) . . . 3_665 ? C9 C10 C11 C2 -0.6(3) . . . . ? C3 C2 C11 C10 0.3(3) . . . . ? C1 C2 C11 C10 -179.37(17) . . . . ? C3 C2 C11 C1 -179.53(16) . . . 3_665 ? C1 C2 C11 C1 0.8(3) . . . 3_665 ? C13 C14 C15 C16 65.0(2) . . . . ? C14 C15 C16 C17 -179.72(18) . . . . ? C28 C18 C19 C20 179.89(17) 3_545 . . . ? C29 C18 C19 C20 0.8(3) . . . . ? C28 C18 C19 C28 -0.4(3) 3_545 . . . ? C29 C18 C19 C28 -179.47(18) . . . . ? C18 C19 C20 C21 179.33(18) . . . . ? C28 C19 C20 C21 -0.4(3) . . . . ? C19 C20 C21 C22 -179.99(18) . . . . ? C19 C20 C21 C26 1.0(3) . . . . ? C20 C21 C22 C23 -179.09(18) . . . . ? C26 C21 C22 C23 -0.1(3) . . . . ? C21 C22 C23 C24 -0.3(3) . . . . ? C22 C23 C24 C25 0.8(3) . . . . ? C23 C24 C25 C26 -0.9(3) . . . . ? C24 C25 C26 C27 -179.61(19) . . . . ? C24 C25 C26 C21 0.6(3) . . . . ? C20 C21 C26 C27 -0.8(3) . . . . ? C22 C21 C26 C27 -179.89(18) . . . . ? C20 C21 C26 C25 178.98(17) . . . . ? C22 C21 C26 C25 -0.1(3) . . . . ? C25 C26 C27 C28 -179.69(18) . . . . ? C21 C26 C27 C28 0.1(3) . . . . ? C26 C27 C28 C18 -179.98(18) . . . 3_545 ? C26 C27 C28 C19 0.4(3) . . . . ? C20 C19 C28 C27 -0.3(3) . . . . ? C18 C19 C28 C27 179.94(16) . . . . ? C20 C19 C28 C18 -179.88(17) . . . 3_545 ? C18 C19 C28 C18 0.4(3) . . . 3_545 ? C30 C31 C32 C33 -67.4(2) . . . . ? C31 C32 C33 C34 171.98(18) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.275 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.046 # Attachment 'k04107.cif' data_k04107 _database_code_depnum_ccdc_archive 'CCDC 671508' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H38' _chemical_formula_sum 'C38 H38' _chemical_formula_weight 494.68 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6368(1) _cell_length_b 8.3446(2) _cell_length_c 13.7421(3) _cell_angle_alpha 105.5261(9) _cell_angle_beta 100.2523(9) _cell_angle_gamma 92.7360(9) _cell_volume 717.92(3) _cell_formula_units_Z 1 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 3280 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 266 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9748 _exptl_absorpt_correction_T_max 0.9987 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\w scans at fixed \c = 55\%' _diffrn_detector_area_resol_mean 18 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 5024 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2513 _reflns_number_gt 1571 _reflns_threshold_expression >2\s(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^)+(0.0755P)^2^] 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 2513 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1343 _refine_ls_wR_factor_gt 0.1145 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3167(2) 0.58226(19) 0.49429(11) 0.0176(4) Uani 1 1 d . . . C2 C 0.3829(2) 0.50182(18) 0.40214(11) 0.0191(4) Uani 1 1 d . . . C3 C 0.2723(2) 0.50037(19) 0.30454(12) 0.0216(4) Uani 1 1 d . . . H3 H 0.1467 0.5504 0.3001 0.026 Uiso 1 1 calc R . . C4 C 0.3407(2) 0.42830(19) 0.21471(12) 0.0219(4) Uani 1 1 d . . . C5 C 0.2314(3) 0.4299(2) 0.11542(12) 0.0294(5) Uani 1 1 d . . . H5 H 0.1049 0.4786 0.1098 0.035 Uiso 1 1 calc R . . C6 C 0.3062(3) 0.3625(2) 0.02893(13) 0.0334(5) Uani 1 1 d . . . H6 H 0.2328 0.3665 -0.0363 0.040 Uiso 1 1 calc R . . C7 C 0.4932(3) 0.2865(2) 0.03558(13) 0.0335(5) Uani 1 1 d . . . H7 H 0.5433 0.2392 -0.0254 0.040 Uiso 1 1 calc R . . C8 C 0.6008(3) 0.2806(2) 0.12776(13) 0.0297(5) Uani 1 1 d . . . H8 H 0.7252 0.2286 0.1305 0.036 Uiso 1 1 calc R . . C9 C 0.5308(2) 0.35123(19) 0.22112(12) 0.0230(4) Uani 1 1 d . . . C10 C 0.6379(2) 0.34780(19) 0.31624(12) 0.0218(4) Uani 1 1 d . . . H10 H 0.7613 0.2946 0.3197 0.026 Uiso 1 1 calc R . . C11 C 0.5707(2) 0.42033(18) 0.40832(11) 0.0179(4) Uani 1 1 d . . . C12 C 0.1360(2) 0.66897(19) 0.48851(11) 0.0202(4) Uani 1 1 d . . . C13 C -0.0122(2) 0.74409(19) 0.48461(11) 0.0199(4) Uani 1 1 d . . . C14 C -0.1981(2) 0.83236(19) 0.47558(11) 0.0197(4) Uani 1 1 d . . . H14A H -0.1649 0.9494 0.5191 0.024 Uiso 1 1 calc R . . H14B H -0.3046 0.7788 0.5020 0.024 Uiso 1 1 calc R . . C15 C -0.2850(2) 0.83215(19) 0.36485(11) 0.0208(4) Uani 1 1 d . . . H15A H -0.1809 0.8903 0.3394 0.025 Uiso 1 1 calc R . . H15B H -0.3127 0.7153 0.3207 0.025 Uiso 1 1 calc R . . C16 C -0.4820(2) 0.91708(19) 0.35567(11) 0.0200(4) Uani 1 1 d . . . H16A H -0.5827 0.8634 0.3854 0.024 Uiso 1 1 calc R . . H16B H -0.4520 1.0357 0.3967 0.024 Uiso 1 1 calc R . . C17 C -0.5783(2) 0.90919(19) 0.24554(11) 0.0224(4) Uani 1 1 d . . . H17A H -0.5981 0.7910 0.2034 0.027 Uiso 1 1 calc R . . H17B H -0.4818 0.9705 0.2176 0.027 Uiso 1 1 calc R . . C18 C -0.7840(2) 0.9823(2) 0.23495(12) 0.0284(5) Uani 1 1 d . . . H18A H -0.7647 1.1004 0.2771 0.034 Uiso 1 1 calc R . . H18B H -0.8811 0.9207 0.2624 0.034 Uiso 1 1 calc R . . C19 C -0.8779(3) 0.9739(2) 0.12388(12) 0.0376(5) Uani 1 1 d . . . H19A H -0.7856 1.0392 0.0973 0.056 Uiso 1 1 calc R . . H19B H -1.0113 1.0198 0.1214 0.056 Uiso 1 1 calc R . . H19C H -0.8972 0.8573 0.0816 0.056 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 C1 0.0159(8) 0.0154(9) 0.0216(9) 0.0063(7) 0.0025(7) 0.0009(7) C2 0.0184(9) 0.0159(9) 0.0230(10) 0.0061(7) 0.0032(7) 0.0012(7) C3 0.0193(9) 0.0192(9) 0.0266(10) 0.0072(7) 0.0030(8) 0.0053(7) C4 0.0249(9) 0.0193(9) 0.0211(9) 0.0063(7) 0.0027(8) 0.0026(7) C5 0.0319(11) 0.0286(10) 0.0278(11) 0.0103(8) 0.0018(8) 0.0065(8) C6 0.0416(11) 0.0369(11) 0.0210(10) 0.0106(8) 0.0001(8) 0.0045(9) C7 0.0425(12) 0.0336(11) 0.0254(10) 0.0064(8) 0.0115(9) 0.0071(9) C8 0.0334(11) 0.0310(11) 0.0271(10) 0.0080(8) 0.0108(8) 0.0106(8) C9 0.0267(10) 0.0193(10) 0.0246(10) 0.0070(7) 0.0073(8) 0.0040(8) C10 0.0214(9) 0.0197(9) 0.0264(10) 0.0073(7) 0.0073(7) 0.0066(7) C11 0.0174(9) 0.0145(9) 0.0223(10) 0.0054(7) 0.0048(7) 0.0028(7) C12 0.0211(9) 0.0190(9) 0.0207(9) 0.0057(7) 0.0044(7) 0.0028(8) C13 0.0227(9) 0.0194(9) 0.0184(9) 0.0056(7) 0.0052(7) 0.0031(8) C14 0.0164(9) 0.0210(10) 0.0237(9) 0.0069(7) 0.0067(7) 0.0061(7) C15 0.0200(9) 0.0221(9) 0.0211(9) 0.0055(7) 0.0060(7) 0.0056(7) C16 0.0191(9) 0.0208(9) 0.0215(9) 0.0068(7) 0.0052(7) 0.0057(7) C17 0.0238(10) 0.0225(10) 0.0225(10) 0.0074(8) 0.0058(8) 0.0056(8) C18 0.0258(10) 0.0343(11) 0.0257(10) 0.0101(8) 0.0028(8) 0.0088(8) C19 0.0337(11) 0.0451(13) 0.0322(11) 0.0119(9) -0.0017(9) 0.0108(9) _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 C1 C11 1.418(2) 2_666 ? C1 C2 1.420(2) . ? C1 C12 1.431(2) . ? C2 C3 1.406(2) . ? C2 C11 1.448(2) . ? C3 C4 1.386(2) . ? C3 H3 0.9500 . ? C4 C5 1.431(2) . ? C4 C9 1.442(2) . ? C5 C6 1.362(2) . ? C5 H5 0.9500 . ? C6 C7 1.421(2) . ? C6 H6 0.9500 . ? C7 C8 1.353(2) . ? C7 H7 0.9500 . ? C8 C9 1.430(2) . ? C8 H8 0.9500 . ? C9 C10 1.381(2) . ? C10 C11 1.408(2) . ? C10 H10 0.9500 . ? C11 C1 1.418(2) 2_666 ? C12 C13 1.193(2) . ? C13 C14 1.470(2) . ? C14 C15 1.5277(18) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.5187(19) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.5170(19) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.521(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.5242(19) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? 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 C11 C1 C2 120.79(14) 2_666 . ? C11 C1 C12 119.79(13) 2_666 . ? C2 C1 C12 119.41(13) . . ? C3 C2 C1 121.90(14) . . ? C3 C2 C11 118.72(14) . . ? C1 C2 C11 119.38(13) . . ? C4 C3 C2 122.13(14) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C3 C4 C5 122.37(15) . . ? C3 C4 C9 119.11(14) . . ? C5 C4 C9 118.50(14) . . ? C6 C5 C4 120.90(16) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 120.40(16) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 120.74(16) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 121.19(15) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 122.44(15) . . ? C10 C9 C4 119.31(14) . . ? C8 C9 C4 118.25(14) . . ? C9 C10 C11 122.35(15) . . ? C9 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C10 C11 C1 121.85(14) . 2_666 ? C10 C11 C2 118.33(14) . . ? C1 C11 C2 119.81(13) 2_666 . ? C13 C12 C1 178.72(17) . . ? C12 C13 C14 177.70(16) . . ? C13 C14 C15 112.85(12) . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C14 112.44(12) . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C17 C16 C15 113.41(12) . . ? C17 C16 H16A 108.9 . . ? C15 C16 H16A 108.9 . . ? C17 C16 H16B 108.9 . . ? C15 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C16 C17 C18 113.67(13) . . ? C16 C17 H17A 108.8 . . ? C18 C17 H17A 108.8 . . ? C16 C17 H17B 108.8 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C17 C18 C19 112.93(13) . . ? C17 C18 H18A 109.0 . . ? C19 C18 H18A 109.0 . . ? C17 C18 H18B 109.0 . . ? C19 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C1 C2 C3 179.00(13) 2_666 . . . ? C12 C1 C2 C3 -2.0(2) . . . . ? C11 C1 C2 C11 -1.7(2) 2_666 . . . ? C12 C1 C2 C11 177.33(13) . . . . ? C1 C2 C3 C4 177.19(14) . . . . ? C11 C2 C3 C4 -2.1(2) . . . . ? C2 C3 C4 C5 -178.50(14) . . . . ? C2 C3 C4 C9 0.4(2) . . . . ? C3 C4 C5 C6 177.92(16) . . . . ? C9 C4 C5 C6 -1.0(2) . . . . ? C4 C5 C6 C7 1.1(3) . . . . ? C5 C6 C7 C8 -0.5(3) . . . . ? C6 C7 C8 C9 -0.3(3) . . . . ? C7 C8 C9 C10 -179.67(15) . . . . ? C7 C8 C9 C4 0.4(2) . . . . ? C3 C4 C9 C10 1.4(2) . . . . ? C5 C4 C9 C10 -179.69(14) . . . . ? C3 C4 C9 C8 -178.74(15) . . . . ? C5 C4 C9 C8 0.2(2) . . . . ? C8 C9 C10 C11 178.72(15) . . . . ? C4 C9 C10 C11 -1.4(2) . . . . ? C9 C10 C11 C1 -179.25(14) . . . 2_666 ? C9 C10 C11 C2 -0.3(2) . . . . ? C3 C2 C11 C10 2.0(2) . . . . ? C1 C2 C11 C10 -177.26(14) . . . . ? C3 C2 C11 C1 -179.00(13) . . . 2_666 ? C1 C2 C11 C1 1.7(2) . . . 2_666 ? C13 C14 C15 C16 177.53(13) . . . . ? C14 C15 C16 C17 -176.50(12) . . . . ? C15 C16 C17 C18 175.61(13) . . . . ? C16 C17 C18 C19 179.77(13) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.300 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.046 # Attachment 'k04111.cif' data_k04111 _database_code_depnum_ccdc_archive 'CCDC 671509' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H34' _chemical_formula_sum 'C36 H34' _chemical_formula_weight 466.63 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3212(3) _cell_length_b 5.1420(2) _cell_length_c 20.8030(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.1599(12) _cell_angle_gamma 90.00 _cell_volume 1293.06(7) _cell_formula_units_Z 2 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 5769 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'thin rod' _exptl_crystal_colour blue _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9716 _exptl_absorpt_correction_T_max 0.9966 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\w scans at fixed \c = 55\%' _diffrn_detector_area_resol_mean 18 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 8382 _diffrn_reflns_av_R_equivalents 0.0923 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2272 _reflns_number_gt 1405 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick,1994)' _computing_publication_material ; SHELX97-2 (Sheldrick, 1997) and local procedures ; _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^)+(0.0676P)^2^] 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 2272 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.51308(16) 0.6924(3) 0.45304(9) 0.0173(5) Uani 1 1 d . . . C2 C 0.59302(15) 0.6709(3) 0.51191(9) 0.0172(5) Uani 1 1 d . . . C3 C 0.68524(16) 0.8370(4) 0.52584(9) 0.0203(5) Uani 1 1 d . . . H3 H 0.6948 0.9647 0.4944 0.024 Uiso 1 1 calc R . . C4 C 0.76261(16) 0.8216(4) 0.58359(9) 0.0186(5) Uani 1 1 d . . . C5 C 0.85579(16) 0.9916(4) 0.59835(10) 0.0230(5) Uani 1 1 d . . . H5 H 0.8660 1.1209 0.5675 0.028 Uiso 1 1 calc R . . C6 C 0.92984(16) 0.9725(4) 0.65542(10) 0.0233(5) Uani 1 1 d . . . H6 H 0.9914 1.0873 0.6641 0.028 Uiso 1 1 calc R . . C7 C 0.91560(17) 0.7800(4) 0.70268(10) 0.0254(5) Uani 1 1 d . . . H7 H 0.9680 0.7678 0.7426 0.031 Uiso 1 1 calc R . . C8 C 0.82877(16) 0.6155(4) 0.69130(10) 0.0232(5) Uani 1 1 d . . . H8 H 0.8208 0.4893 0.7234 0.028 Uiso 1 1 calc R . . C9 C 0.74823(16) 0.6280(4) 0.63155(9) 0.0191(5) Uani 1 1 d . . . C10 C 0.65873(16) 0.4610(4) 0.61796(9) 0.0197(5) Uani 1 1 d . . . H10 H 0.6506 0.3318 0.6493 0.024 Uiso 1 1 calc R . . C11 C 0.57925(15) 0.4749(4) 0.55950(9) 0.0178(5) Uani 1 1 d . . . C12 C 0.52704(16) 0.8852(4) 0.40570(10) 0.0197(5) Uani 1 1 d . . . C13 C 0.53886(15) 1.0482(4) 0.36626(9) 0.0199(5) Uani 1 1 d . . . C14 C 0.55413(16) 1.2466(4) 0.31833(9) 0.0218(5) Uani 1 1 d . . . H14A H 0.5520 1.4207 0.3384 0.026 Uiso 1 1 calc R . . H14B H 0.4920 1.2364 0.2803 0.026 Uiso 1 1 calc R . . C15 C 0.66353(16) 1.2163(4) 0.29431(9) 0.0250(5) Uani 1 1 d . . . H15A H 0.6642 1.0439 0.2732 0.030 Uiso 1 1 calc R . . H15B H 0.6667 1.3500 0.2605 0.030 Uiso 1 1 calc R . . C16 C 0.76687(16) 1.2404(4) 0.34758(9) 0.0248(5) Uani 1 1 d . . . H16A H 0.7635 1.1079 0.3817 0.030 Uiso 1 1 calc R . . H16B H 0.8324 1.2014 0.3282 0.030 Uiso 1 1 calc R . . C17 C 0.78237(16) 1.5054(4) 0.37989(10) 0.0285(6) Uani 1 1 d . . . H17A H 0.7201 1.5391 0.4025 0.034 Uiso 1 1 calc R . . H17B H 0.7803 1.6399 0.3456 0.034 Uiso 1 1 calc R . . C18 C 0.89100(17) 1.5294(4) 0.42930(11) 0.0372(6) Uani 1 1 d . . . H18A H 0.8921 1.4026 0.4646 0.056 Uiso 1 1 calc R . . H18B H 0.8976 1.7054 0.4477 0.056 Uiso 1 1 calc R . . H18C H 0.9531 1.4956 0.4073 0.056 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 C1 0.0203(11) 0.0169(11) 0.0158(12) -0.0005(9) 0.0062(9) 0.0019(9) C2 0.0192(11) 0.0188(12) 0.0139(12) -0.0035(9) 0.0041(9) 0.0013(9) C3 0.0239(12) 0.0207(12) 0.0176(12) 0.0003(9) 0.0073(10) -0.0005(10) C4 0.0195(11) 0.0204(12) 0.0156(12) -0.0031(9) 0.0029(9) 0.0019(9) C5 0.0245(12) 0.0232(12) 0.0210(13) -0.0013(10) 0.0038(10) -0.0003(10) C6 0.0206(12) 0.0218(12) 0.0265(13) -0.0025(10) 0.0021(10) -0.0018(10) C7 0.0248(12) 0.0284(13) 0.0207(13) -0.0035(11) -0.0016(10) 0.0035(11) C8 0.0259(12) 0.0243(12) 0.0177(12) 0.0025(10) -0.0001(10) 0.0025(10) C9 0.0201(12) 0.0211(11) 0.0166(12) -0.0016(9) 0.0047(9) 0.0039(10) C10 0.0229(12) 0.0203(12) 0.0165(12) 0.0025(9) 0.0048(9) 0.0038(9) C11 0.0199(12) 0.0180(11) 0.0156(11) -0.0024(9) 0.0039(9) 0.0030(10) C12 0.0166(11) 0.0224(12) 0.0191(12) -0.0028(10) 0.0014(9) 0.0006(9) C13 0.0177(11) 0.0243(12) 0.0158(12) -0.0026(10) -0.0015(9) 0.0011(10) C14 0.0267(12) 0.0195(11) 0.0182(12) 0.0018(10) 0.0020(9) -0.0005(10) C15 0.0284(12) 0.0262(12) 0.0219(13) 0.0000(10) 0.0086(10) -0.0008(10) C16 0.0234(12) 0.0262(13) 0.0262(13) 0.0035(10) 0.0077(10) 0.0012(10) C17 0.0290(13) 0.0337(13) 0.0225(13) -0.0016(10) 0.0039(10) 0.0017(11) C18 0.0335(14) 0.0415(15) 0.0335(15) -0.0034(12) -0.0010(11) -0.0016(12) _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 C1 C11 1.410(3) 3_666 ? C1 C2 1.419(2) . ? C1 C12 1.431(3) . ? C2 C3 1.406(3) . ? C2 C11 1.446(3) . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.429(3) . ? C4 C9 1.444(3) . ? C5 C6 1.354(3) . ? C5 H5 0.9500 . ? C6 C7 1.430(3) . ? C6 H6 0.9500 . ? C7 C8 1.348(3) . ? C7 H7 0.9500 . ? C8 C9 1.434(3) . ? C8 H8 0.9500 . ? C9 C10 1.383(3) . ? C10 C11 1.408(2) . ? C10 H10 0.9500 . ? C11 C1 1.410(3) 3_666 ? C12 C13 1.201(3) . ? C13 C14 1.464(3) . ? C14 C15 1.534(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.523(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.515(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.527(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 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 C11 C1 C2 120.83(17) 3_666 . ? C11 C1 C12 119.71(17) 3_666 . ? C2 C1 C12 119.46(17) . . ? C3 C2 C1 121.92(18) . . ? C3 C2 C11 118.65(17) . . ? C1 C2 C11 119.42(17) . . ? C4 C3 C2 122.53(18) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 122.79(18) . . ? C3 C4 C9 118.89(17) . . ? C5 C4 C9 118.31(17) . . ? C6 C5 C4 121.42(19) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 120.12(19) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 120.82(19) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 121.10(19) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 122.67(18) . . ? C10 C9 C4 119.10(17) . . ? C8 C9 C4 118.22(18) . . ? C9 C10 C11 122.60(18) . . ? C9 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C10 C11 C1 122.04(18) . 3_666 ? C10 C11 C2 118.21(17) . . ? C1 C11 C2 119.74(17) 3_666 . ? C13 C12 C1 179.6(2) . . ? C12 C13 C14 179.6(2) . . ? C13 C14 C15 112.82(16) . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C14 114.74(16) . . ? C16 C15 H15A 108.6 . . ? C14 C15 H15A 108.6 . . ? C16 C15 H15B 108.6 . . ? C14 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? C17 C16 C15 114.33(16) . . ? C17 C16 H16A 108.7 . . ? C15 C16 H16A 108.7 . . ? C17 C16 H16B 108.7 . . ? C15 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C16 C17 C18 112.97(17) . . ? C16 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? C16 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C1 C2 C3 -179.40(18) 3_666 . . . ? C12 C1 C2 C3 1.1(3) . . . . ? C11 C1 C2 C11 0.0(3) 3_666 . . . ? C12 C1 C2 C11 -179.57(17) . . . . ? C1 C2 C3 C4 178.69(17) . . . . ? C11 C2 C3 C4 -0.7(3) . . . . ? C2 C3 C4 C5 -179.26(18) . . . . ? C2 C3 C4 C9 -0.1(3) . . . . ? C3 C4 C5 C6 179.69(18) . . . . ? C9 C4 C5 C6 0.5(3) . . . . ? C4 C5 C6 C7 -0.3(3) . . . . ? C5 C6 C7 C8 0.0(3) . . . . ? C6 C7 C8 C9 0.1(3) . . . . ? C7 C8 C9 C10 179.39(19) . . . . ? C7 C8 C9 C4 0.1(3) . . . . ? C3 C4 C9 C10 1.1(3) . . . . ? C5 C4 C9 C10 -179.74(18) . . . . ? C3 C4 C9 C8 -179.64(17) . . . . ? C5 C4 C9 C8 -0.5(3) . . . . ? C8 C9 C10 C11 179.47(18) . . . . ? C4 C9 C10 C11 -1.3(3) . . . . ? C9 C10 C11 C1 -178.41(18) . . . 3_666 ? C9 C10 C11 C2 0.5(3) . . . . ? C3 C2 C11 C10 0.5(3) . . . . ? C1 C2 C11 C10 -178.88(16) . . . . ? C3 C2 C11 C1 179.42(17) . . . 3_666 ? C1 C2 C11 C1 0.0(3) . . . 3_666 ? C13 C14 C15 C16 -61.3(2) . . . . ? C14 C15 C16 C17 -63.8(2) . . . . ? C15 C16 C17 C18 -175.62(17) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.193 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.048 # Attachment 'k04197.cif' data_k04197 _database_code_depnum_ccdc_archive 'CCDC 671510' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H74 Si2' _chemical_formula_sum 'C54 H74 Si2' _chemical_formula_weight 779.31 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' Si Si .0817 .0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8577(1) _cell_length_b 11.1290(1) _cell_length_c 12.5975(1) _cell_angle_alpha 101.9194(4) _cell_angle_beta 93.8211(4) _cell_angle_gamma 101.2905(4) _cell_volume 1184.09(2) _cell_formula_units_Z 1 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 5344 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'irregular block' _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 426 _exptl_absorpt_coefficient_mu 0.109 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9733 _exptl_absorpt_correction_T_max 0.9807 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\w scans at fixed \c = 55\%' _diffrn_detector_area_resol_mean 18 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 10620 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5412 _reflns_number_gt 4728 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 1994)' _computing_publication_material ; SHELX97-2 (Sheldrick, 1997) and local procedures ; _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 octyl group is disordered but it was easy to model. ; _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^)+(0.0597P)^2^+0.3274P] 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 5412 _refine_ls_number_parameters 288 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1053 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 1.05787(3) 0.73079(3) 0.35243(2) 0.01457(9) Uani 1 1 d . . . C1 C 1.02247(12) 0.93825(10) 0.08603(8) 0.0166(2) Uani 1 1 d . . . C2 C 0.91145(12) 0.87634(10) -0.00495(8) 0.0161(2) Uani 1 1 d . . . C3 C 0.82294(12) 0.75415(10) -0.01343(9) 0.0181(2) Uani 1 1 d . . . H3 H 0.8381 0.7120 0.0435 0.022 Uiso 1 1 calc R . . C4 C 0.71457(12) 0.69373(10) -0.10214(9) 0.0180(2) Uani 1 1 d . . . C5 C 0.62582(13) 0.56839(11) -0.11197(10) 0.0213(2) Uani 1 1 d . . . H5 H 0.6406 0.5250 -0.0559 0.026 Uiso 1 1 calc R . . C6 C 0.52098(13) 0.51110(11) -0.20048(10) 0.0231(2) Uani 1 1 d . . . H6 H 0.4636 0.4281 -0.2057 0.028 Uiso 1 1 calc R . . C7 C 0.49634(13) 0.57462(11) -0.28563(10) 0.0227(2) Uani 1 1 d . . . H7 H 0.4223 0.5335 -0.3468 0.027 Uiso 1 1 calc R . . C8 C 0.57751(13) 0.69301(11) -0.28005(9) 0.0204(2) Uani 1 1 d . . . H8 H 0.5596 0.7339 -0.3374 0.024 Uiso 1 1 calc R . . C9 C 0.69001(12) 0.75718(10) -0.18859(9) 0.0174(2) Uani 1 1 d . . . C10 C 0.77589(12) 0.87766(10) -0.18124(9) 0.0170(2) Uani 1 1 d . . . H10 H 0.7587 0.9196 -0.2380 0.020 Uiso 1 1 calc R . . C11 C 0.88798(12) 0.93968(10) -0.09193(8) 0.0158(2) Uani 1 1 d . . . C12 C 1.04269(12) 0.87636(10) 0.17309(9) 0.0183(2) Uani 1 1 d . . . C13 C 1.05569(13) 0.82331(11) 0.24674(9) 0.0198(2) Uani 1 1 d . A . C14 C 1.26577(12) 0.72463(10) 0.38799(9) 0.0186(2) Uani 1 1 d . A . H14 H 1.3101 0.7038 0.3172 0.022 Uiso 1 1 calc R . . C15 C 1.36086(14) 0.85369(12) 0.44964(11) 0.0291(3) Uani 1 1 d . . . H15A H 1.3251 0.8762 0.5216 0.044 Uiso 1 1 calc R A . H15B H 1.3476 0.9170 0.4081 0.044 Uiso 1 1 calc R . . H15C H 1.4706 0.8503 0.4586 0.044 Uiso 1 1 calc R . . C16 C 1.28656(16) 0.62225(13) 0.44898(11) 0.0322(3) Uani 1 1 d . . . H16A H 1.3968 0.6209 0.4597 0.048 Uiso 1 1 calc R A . H16B H 1.2291 0.5403 0.4062 0.048 Uiso 1 1 calc R . . H16C H 1.2471 0.6400 0.5201 0.048 Uiso 1 1 calc R . . C17 C 0.96968(13) 0.81251(11) 0.47108(9) 0.0202(2) Uani 1 1 d . A . H17 H 1.0365 0.8986 0.4976 0.024 Uiso 1 1 calc R . . C18 C 0.9686(2) 0.74804(19) 0.56651(13) 0.0549(5) Uani 1 1 d . . . H18A H 0.9221 0.7942 0.6260 0.082 Uiso 1 1 calc R A . H18B H 1.0751 0.7468 0.5921 0.082 Uiso 1 1 calc R . . H18C H 0.9079 0.6616 0.5429 0.082 Uiso 1 1 calc R . . C19 C 0.80731(15) 0.82927(14) 0.43807(12) 0.0339(3) Uani 1 1 d . . . H19A H 0.7375 0.7466 0.4127 0.051 Uiso 1 1 calc R A . H19B H 0.8110 0.8748 0.3792 0.051 Uiso 1 1 calc R . . H19C H 0.7692 0.8772 0.5011 0.051 Uiso 1 1 calc R . . C20 C 0.93478(13) 0.57219(11) 0.28971(9) 0.0212(2) Uani 0.8836(18) 1 d PD A 1 H20A H 0.9376 0.5177 0.3425 0.025 Uiso 0.8836(18) 1 calc PR A 1 H20B H 0.8263 0.5808 0.2768 0.025 Uiso 0.8836(18) 1 calc PR A 1 C21 C 0.98356(15) 0.50614(12) 0.18072(11) 0.0208(3) Uani 0.8836(18) 1 d PD A 1 H21A H 1.0009 0.5666 0.1328 0.025 Uiso 0.8836(18) 1 calc PR A 1 H21B H 1.0830 0.4816 0.1958 0.025 Uiso 0.8836(18) 1 calc PR A 1 C22 C 0.86327(16) 0.38897(12) 0.12023(11) 0.0204(3) Uani 0.8836(18) 1 d PD A 1 H22A H 0.7639 0.4137 0.1052 0.024 Uiso 0.8836(18) 1 calc PR A 1 H22B H 0.8982 0.3556 0.0491 0.024 Uiso 0.8836(18) 1 calc PR A 1 C23 C 0.83576(15) 0.28493(12) 0.18304(10) 0.0192(3) Uani 0.8836(18) 1 d PD A 1 H23A H 0.8020 0.3184 0.2545 0.023 Uiso 0.8836(18) 1 calc PR A 1 H23B H 0.9347 0.2592 0.1971 0.023 Uiso 0.8836(18) 1 calc PR A 1 C24 C 0.71452(14) 0.16982(11) 0.12284(10) 0.0192(3) Uani 0.8836(18) 1 d PD A 1 H24A H 0.7486 0.1365 0.0514 0.023 Uiso 0.8836(18) 1 calc PR A 1 H24B H 0.6159 0.1959 0.1085 0.023 Uiso 0.8836(18) 1 calc PR A 1 C25 C 0.68515(15) 0.06486(12) 0.18481(10) 0.0208(3) Uani 0.8836(18) 1 d PD A 1 H25A H 0.6481 0.0970 0.2554 0.025 Uiso 0.8836(18) 1 calc PR A 1 H25B H 0.7839 0.0396 0.2006 0.025 Uiso 0.8836(18) 1 calc PR A 1 C26 C 0.5657(2) -0.05063(19) 0.12100(14) 0.0219(3) Uani 0.8836(18) 1 d PD A 1 H26A H 0.4646 -0.0267 0.1109 0.026 Uiso 0.8836(18) 1 calc PR A 1 H26B H 0.5981 -0.0777 0.0477 0.026 Uiso 0.8836(18) 1 calc PR A 1 C27 C 0.54476(18) -0.16097(14) 0.17662(13) 0.0318(3) Uani 0.8836(18) 1 d PD A 1 H27A H 0.6427 -0.1887 0.1830 0.048 Uiso 0.8836(18) 1 calc PR A 1 H27B H 0.4645 -0.2304 0.1331 0.048 Uiso 0.8836(18) 1 calc PR A 1 H27C H 0.5136 -0.1348 0.2496 0.048 Uiso 0.8836(18) 1 calc PR A 1 C20' C 0.93478(13) 0.57219(11) 0.28971(9) 0.0212(2) Uani 0.1164(18) 1 d PD A 2 H20C H 0.8847 0.5383 0.3485 0.025 Uiso 0.1164(18) 1 calc PR A 2 H20D H 0.8513 0.5831 0.2386 0.025 Uiso 0.1164(18) 1 calc PR A 2 C21' C 1.0159(10) 0.4715(8) 0.2269(8) 0.016(2) Uiso 0.1164(18) 1 d PD A 2 H21C H 1.0970 0.4565 0.2775 0.020 Uiso 0.1164(18) 1 calc PR A 2 H21D H 1.0671 0.5038 0.1678 0.020 Uiso 0.1164(18) 1 calc PR A 2 C22' C 0.8999(12) 0.3450(10) 0.1766(8) 0.021(2) Uiso 0.1164(18) 1 d PD A 2 H22C H 0.9588 0.2779 0.1590 0.025 Uiso 0.1164(18) 1 calc PR A 2 H22D H 0.8314 0.3238 0.2321 0.025 Uiso 0.1164(18) 1 calc PR A 2 C23' C 0.8005(11) 0.3461(9) 0.0747(8) 0.019(2) Uiso 0.1164(18) 1 d PD A 2 H23C H 0.8672 0.3591 0.0162 0.023 Uiso 0.1164(18) 1 calc PR A 2 H23D H 0.7465 0.4167 0.0899 0.023 Uiso 0.1164(18) 1 calc PR A 2 C24' C 0.6801(10) 0.2211(8) 0.0359(7) 0.018(2) Uiso 0.1164(18) 1 d PD A 2 H24C H 0.7344 0.1505 0.0269 0.021 Uiso 0.1164(18) 1 calc PR A 2 H24D H 0.6095 0.2116 0.0928 0.021 Uiso 0.1164(18) 1 calc PR A 2 C25' C 0.5848(10) 0.2131(8) -0.0710(7) 0.018(2) Uiso 0.1164(18) 1 d PD A 2 H25C H 0.6557 0.2255 -0.1272 0.022 Uiso 0.1164(18) 1 calc PR A 2 H25D H 0.5280 0.2822 -0.0612 0.022 Uiso 0.1164(18) 1 calc PR A 2 C26' C 0.4666(19) 0.0857(15) -0.1127(14) 0.035(5) Uiso 0.1164(18) 1 d PD A 2 H26C H 0.5246 0.0175 -0.1250 0.042 Uiso 0.1164(18) 1 calc PR A 2 H26D H 0.3997 0.0718 -0.0545 0.042 Uiso 0.1164(18) 1 calc PR A 2 C27' C 0.3664(14) 0.0757(12) -0.2141(10) 0.038(3) Uiso 0.1164(18) 1 d PD A 2 H27D H 0.3041 0.1400 -0.2021 0.057 Uiso 0.1164(18) 1 calc PR A 2 H27E H 0.2976 -0.0079 -0.2347 0.057 Uiso 0.1164(18) 1 calc PR A 2 H27F H 0.4309 0.0882 -0.2728 0.057 Uiso 0.1164(18) 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 0.01538(15) 0.01418(16) 0.01418(15) 0.00511(11) 0.00062(11) 0.00159(11) C1 0.0179(5) 0.0199(5) 0.0153(5) 0.0068(4) 0.0050(4) 0.0076(4) C2 0.0171(5) 0.0182(5) 0.0157(5) 0.0057(4) 0.0051(4) 0.0072(4) C3 0.0190(5) 0.0209(6) 0.0181(5) 0.0088(4) 0.0051(4) 0.0075(4) C4 0.0162(5) 0.0202(5) 0.0202(5) 0.0066(4) 0.0049(4) 0.0069(4) C5 0.0197(5) 0.0212(6) 0.0254(6) 0.0092(5) 0.0039(4) 0.0053(4) C6 0.0190(5) 0.0201(6) 0.0302(6) 0.0068(5) 0.0031(5) 0.0026(4) C7 0.0183(5) 0.0249(6) 0.0230(6) 0.0019(5) 0.0003(4) 0.0042(4) C8 0.0197(5) 0.0241(6) 0.0184(5) 0.0054(4) 0.0022(4) 0.0066(4) C9 0.0166(5) 0.0210(5) 0.0168(5) 0.0049(4) 0.0047(4) 0.0075(4) C10 0.0184(5) 0.0205(5) 0.0149(5) 0.0064(4) 0.0037(4) 0.0076(4) C11 0.0162(5) 0.0191(5) 0.0149(5) 0.0053(4) 0.0050(4) 0.0076(4) C12 0.0175(5) 0.0193(5) 0.0181(5) 0.0050(4) 0.0020(4) 0.0033(4) C13 0.0193(5) 0.0200(6) 0.0192(5) 0.0059(4) -0.0004(4) 0.0014(4) C14 0.0168(5) 0.0212(6) 0.0181(5) 0.0046(4) 0.0019(4) 0.0048(4) C15 0.0172(6) 0.0297(7) 0.0336(7) -0.0036(5) -0.0016(5) 0.0015(5) C16 0.0312(7) 0.0394(8) 0.0357(7) 0.0188(6) 0.0054(5) 0.0187(6) C17 0.0197(5) 0.0207(6) 0.0197(5) 0.0027(4) 0.0021(4) 0.0051(4) C18 0.0802(13) 0.0798(13) 0.0327(8) 0.0316(8) 0.0344(8) 0.0541(11) C19 0.0233(6) 0.0392(8) 0.0371(7) -0.0013(6) 0.0024(5) 0.0124(6) C20 0.0194(5) 0.0170(5) 0.0242(6) 0.0012(4) 0.0044(4) -0.0004(4) C21 0.0222(6) 0.0174(6) 0.0211(6) 0.0031(5) 0.0042(5) 0.0010(5) C22 0.0223(6) 0.0198(6) 0.0180(6) 0.0029(5) 0.0020(5) 0.0034(5) C23 0.0202(6) 0.0172(6) 0.0187(6) 0.0021(5) 0.0013(5) 0.0029(5) C24 0.0192(6) 0.0173(6) 0.0194(6) 0.0016(5) 0.0027(5) 0.0020(5) C25 0.0214(6) 0.0194(6) 0.0201(6) 0.0029(5) 0.0019(5) 0.0030(5) C26 0.0221(8) 0.0200(9) 0.0236(8) 0.0062(6) 0.0032(6) 0.0032(8) C27 0.0359(8) 0.0251(7) 0.0333(8) 0.0112(6) 0.0035(6) -0.0010(6) C20' 0.0194(5) 0.0170(5) 0.0242(6) 0.0012(4) 0.0044(4) -0.0004(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 C13 1.8450(12) . ? Si1 C20 1.8666(11) . ? Si1 C17 1.8826(11) . ? Si1 C14 1.8838(11) . ? C1 C11 1.4174(15) 2_775 ? C1 C2 1.4190(15) . ? C1 C12 1.4295(14) . ? C2 C3 1.4095(15) . ? C2 C11 1.4446(14) . ? C3 C4 1.3843(16) . ? C3 H3 0.9500 . ? C4 C5 1.4372(15) . ? C4 C9 1.4417(15) . ? C5 C6 1.3596(17) . ? C5 H5 0.9500 . ? C6 C7 1.4284(16) . ? C6 H6 0.9500 . ? C7 C8 1.3572(16) . ? C7 H7 0.9500 . ? C8 C9 1.4349(15) . ? C8 H8 0.9500 . ? C9 C10 1.3874(15) . ? C10 C11 1.4106(15) . ? C10 H10 0.9500 . ? C11 C1 1.4173(15) 2_775 ? C12 C13 1.2088(16) . ? C14 C16 1.5321(16) . ? C14 C15 1.5343(16) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.5216(18) . ? C17 C19 1.5277(17) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.5488(16) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.5342(18) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.5230(18) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.5235(17) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.5252(17) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.532(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.522(2) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C21' C22' 1.555(11) . ? C21' H21C 0.9900 . ? C21' H21D 0.9900 . ? C22' C23' 1.511(11) . ? C22' H22C 0.9900 . ? C22' H22D 0.9900 . ? C23' C24' 1.543(11) . ? C23' H23C 0.9900 . ? C23' H23D 0.9900 . ? C24' C25' 1.518(10) . ? C24' H24C 0.9900 . ? C24' H24D 0.9900 . ? C25' C26' 1.556(13) . ? C25' H25C 0.9900 . ? C25' H25D 0.9900 . ? C26' C27' 1.478(15) . ? C26' H26C 0.9900 . ? C26' H26D 0.9900 . ? C27' H27D 0.9800 . ? C27' H27E 0.9800 . ? C27' H27F 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 C13 Si1 C20 105.95(5) . . ? C13 Si1 C17 106.95(5) . . ? C20 Si1 C17 110.83(5) . . ? C13 Si1 C14 107.14(5) . . ? C20 Si1 C14 112.36(5) . . ? C17 Si1 C14 113.12(5) . . ? C11 C1 C2 120.97(10) 2_775 . ? C11 C1 C12 119.87(10) 2_775 . ? C2 C1 C12 119.16(10) . . ? C3 C2 C1 121.96(10) . . ? C3 C2 C11 118.66(10) . . ? C1 C2 C11 119.38(10) . . ? C4 C3 C2 121.99(10) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 122.19(10) . . ? C3 C4 C9 119.44(10) . . ? C5 C4 C9 118.37(10) . . ? C6 C5 C4 120.86(11) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 120.59(11) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 120.71(11) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 120.79(11) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 122.07(10) . . ? C10 C9 C4 119.24(10) . . ? C8 C9 C4 118.69(10) . . ? C9 C10 C11 121.88(10) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C10 C11 C1 121.58(10) . 2_775 ? C10 C11 C2 118.78(10) . . ? C1 C11 C2 119.64(10) 2_775 . ? C13 C12 C1 178.31(12) . . ? C12 C13 Si1 174.26(10) . . ? C16 C14 C15 111.10(10) . . ? C16 C14 Si1 114.38(8) . . ? C15 C14 Si1 111.34(8) . . ? C16 C14 H14 106.5 . . ? C15 C14 H14 106.5 . . ? Si1 C14 H14 106.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C19 110.51(11) . . ? C18 C17 Si1 112.66(9) . . ? C19 C17 Si1 112.45(8) . . ? C18 C17 H17 106.9 . . ? C19 C17 H17 106.9 . . ? Si1 C17 H17 106.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 Si1 114.65(8) . . ? C21 C20 H20A 108.6 . . ? Si1 C20 H20A 108.6 . . ? C21 C20 H20B 108.6 . . ? Si1 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C22 C21 C20 113.31(10) . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21B 108.9 . . ? C20 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C23 C22 C21 113.65(11) . . ? C23 C22 H22A 108.8 . . ? C21 C22 H22A 108.8 . . ? C23 C22 H22B 108.8 . . ? C21 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C22 C23 C24 113.16(11) . . ? C22 C23 H23A 108.9 . . ? C24 C23 H23A 108.9 . . ? C22 C23 H23B 108.9 . . ? C24 C23 H23B 108.9 . . ? H23A C23 H23B 107.8 . . ? C23 C24 C25 113.84(10) . . ? C23 C24 H24A 108.8 . . ? C25 C24 H24A 108.8 . . ? C23 C24 H24B 108.8 . . ? C25 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C24 C25 C26 112.56(11) . . ? C24 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? C24 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C27 C26 C25 113.55(13) . . ? C27 C26 H26A 108.9 . . ? C25 C26 H26A 108.9 . . ? C27 C26 H26B 108.9 . . ? C25 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? C22' C21' H21C 109.2 . . ? C22' C21' H21D 109.2 . . ? H21C C21' H21D 107.9 . . ? C23' C22' C21' 114.2(9) . . ? C23' C22' H22C 108.7 . . ? C21' C22' H22C 108.7 . . ? C23' C22' H22D 108.7 . . ? C21' C22' H22D 108.7 . . ? H22C C22' H22D 107.6 . . ? C22' C23' C24' 110.7(8) . . ? C22' C23' H23C 109.5 . . ? C24' C23' H23C 109.5 . . ? C22' C23' H23D 109.5 . . ? C24' C23' H23D 109.5 . . ? H23C C23' H23D 108.1 . . ? C25' C24' C23' 113.0(7) . . ? C25' C24' H24C 109.0 . . ? C23' C24' H24C 109.0 . . ? C25' C24' H24D 109.0 . . ? C23' C24' H24D 109.0 . . ? H24C C24' H24D 107.8 . . ? C24' C25' C26' 113.4(9) . . ? C24' C25' H25C 108.9 . . ? C26' C25' H25C 108.9 . . ? C24' C25' H25D 108.9 . . ? C26' C25' H25D 108.9 . . ? H25C C25' H25D 107.7 . . ? C27' C26' C25' 115.3(12) . . ? C27' C26' H26C 108.4 . . ? C25' C26' H26C 108.4 . . ? C27' C26' H26D 108.4 . . ? C25' C26' H26D 108.4 . . ? H26C C26' H26D 107.5 . . ? C26' C27' H27D 109.5 . . ? C26' C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? C26' C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C1 C2 C3 178.93(9) 2_775 . . . ? C12 C1 C2 C3 -1.59(16) . . . . ? C11 C1 C2 C11 -0.94(17) 2_775 . . . ? C12 C1 C2 C11 178.54(9) . . . . ? C1 C2 C3 C4 179.97(10) . . . . ? C11 C2 C3 C4 -0.17(16) . . . . ? C2 C3 C4 C5 178.99(10) . . . . ? C2 C3 C4 C9 -0.36(16) . . . . ? C3 C4 C5 C6 -179.51(11) . . . . ? C9 C4 C5 C6 -0.15(16) . . . . ? C4 C5 C6 C7 -0.23(17) . . . . ? C5 C6 C7 C8 0.30(18) . . . . ? C6 C7 C8 C9 0.03(17) . . . . ? C7 C8 C9 C10 179.28(10) . . . . ? C7 C8 C9 C4 -0.41(16) . . . . ? C3 C4 C9 C10 0.14(15) . . . . ? C5 C4 C9 C10 -179.23(10) . . . . ? C3 C4 C9 C8 179.84(10) . . . . ? C5 C4 C9 C8 0.46(15) . . . . ? C8 C9 C10 C11 -179.06(10) . . . . ? C4 C9 C10 C11 0.63(16) . . . . ? C9 C10 C11 C1 178.70(9) . . . 2_775 ? C9 C10 C11 C2 -1.15(16) . . . . ? C3 C2 C11 C10 0.91(15) . . . . ? C1 C2 C11 C10 -179.22(9) . . . . ? C3 C2 C11 C1 -178.95(9) . . . 2_775 ? C1 C2 C11 C1 0.92(17) . . . 2_775 ? C13 Si1 C14 C16 -163.31(9) . . . . ? C20 Si1 C14 C16 -47.34(10) . . . . ? C17 Si1 C14 C16 79.08(10) . . . . ? C13 Si1 C14 C15 69.72(9) . . . . ? C20 Si1 C14 C15 -174.31(8) . . . . ? C17 Si1 C14 C15 -47.90(10) . . . . ? C13 Si1 C17 C18 -178.22(11) . . . . ? C20 Si1 C17 C18 66.73(12) . . . . ? C14 Si1 C17 C18 -60.49(12) . . . . ? C13 Si1 C17 C19 56.10(10) . . . . ? C20 Si1 C17 C19 -58.95(10) . . . . ? C14 Si1 C17 C19 173.82(9) . . . . ? C13 Si1 C20 C21 55.15(10) . . . . ? C17 Si1 C20 C21 170.82(9) . . . . ? C14 Si1 C20 C21 -61.54(10) . . . . ? Si1 C20 C21 C22 -168.74(9) . . . . ? C20 C21 C22 C23 -62.84(15) . . . . ? C21 C22 C23 C24 179.21(10) . . . . ? C22 C23 C24 C25 -179.81(10) . . . . ? C23 C24 C25 C26 -178.63(12) . . . . ? C24 C25 C26 C27 174.91(12) . . . . ? C21' C22' C23' C24' -175.3(8) . . . . ? C22' C23' C24' C25' -175.7(8) . . . . ? C23' C24' C25' C26' 178.2(11) . . . . ? C24' C25' C26' C27' 177.4(12) . . . . ? _diffrn_measured_fraction_theta_max .997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full .997 _refine_diff_density_max .323 _refine_diff_density_min -.256 _refine_diff_density_rms .042 # Attachment 'k04226.cif' data_k04226 _database_code_depnum_ccdc_archive 'CCDC 671511' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H58 Si2' _chemical_formula_sum 'C46 H58 Si2' _chemical_formula_weight 667.10 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' Si Si .0817 .0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 8.8840(2) _cell_length_b 22.3240(5) _cell_length_c 10.7970(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.146(1) _cell_angle_gamma 90.00 _cell_volume 2010.32(9) _cell_formula_units_Z 2 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 4721 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'irregular lath' _exptl_crystal_colour 'deep blue' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9544 _exptl_absorpt_correction_T_max 0.9941 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\w scans at fixed \c = 55\%' _diffrn_detector_area_resol_mean 18 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 8955 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0739 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4610 _reflns_number_gt 2931 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 1994)' _computing_publication_material ; SHELX97-2 (Sheldrick, 1997) and local procedures ; _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^)+(0.0644P)^2^+0.0679P] 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 4610 _refine_ls_number_parameters 222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1331 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _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 0.58076(6) 0.18214(2) 0.41301(5) 0.02184(16) Uani 1 1 d . . . C1 C 0.5154(2) 0.04286(8) 0.10100(16) 0.0175(4) Uani 1 1 d . . . C2 C 0.6288(2) 0.04216(7) 0.03425(17) 0.0175(4) Uani 1 1 d . . . C3 C 0.7574(2) 0.08286(7) 0.06654(18) 0.0201(4) Uani 1 1 d . . . H3 H 0.7706 0.1105 0.1364 0.024 Uiso 1 1 calc R . . C4 C 0.8653(2) 0.08396(8) -0.00021(18) 0.0199(4) Uani 1 1 d . . . C5 C 0.9953(2) 0.12518(8) 0.03257(19) 0.0245(4) Uani 1 1 d . . . H5 H 1.0095 0.1529 0.1024 0.029 Uiso 1 1 calc R . . C6 C 1.0991(2) 0.12547(9) -0.0343(2) 0.0281(5) Uani 1 1 d . . . H6 H 1.1856 0.1532 -0.0107 0.034 Uiso 1 1 calc R . . C7 C 1.0798(2) 0.08460(8) -0.13950(19) 0.0262(5) Uani 1 1 d . . . H7 H 1.1533 0.0856 -0.1858 0.031 Uiso 1 1 calc R . . C8 C 0.9590(2) 0.04434(9) -0.17496(18) 0.0240(4) Uani 1 1 d . . . H8 H 0.9484 0.0174 -0.2456 0.029 Uiso 1 1 calc R . . C9 C 0.8459(2) 0.04199(8) -0.10620(17) 0.0199(4) Uani 1 1 d . . . C10 C 0.7219(2) 0.00066(8) -0.13704(17) 0.0192(4) Uani 1 1 d . . . H10 H 0.7109 -0.0274 -0.2057 0.023 Uiso 1 1 calc R . . C11 C 0.6113(2) -0.00079(8) -0.06915(17) 0.0177(4) Uani 1 1 d . . . C12 C 0.5314(2) 0.08700(8) 0.20024(17) 0.0198(4) Uani 1 1 d . . . C13 C 0.5473(2) 0.12519(8) 0.28317(18) 0.0214(4) Uani 1 1 d . . . C14 C 0.7955(2) 0.20664(9) 0.45755(19) 0.0276(5) Uani 1 1 d . . . H14 H 0.8183 0.2361 0.5315 0.033 Uiso 1 1 calc R . . C15 C 0.9127(2) 0.15434(10) 0.5055(2) 0.0430(6) Uani 1 1 d . . . H15A H 0.8921 0.1244 0.4351 0.064 Uiso 1 1 calc R . . H15B H 0.8983 0.1360 0.5831 0.064 Uiso 1 1 calc R . . H15C H 1.0229 0.1691 0.5290 0.064 Uiso 1 1 calc R . . C16 C 0.8237(2) 0.23844(9) 0.3413(2) 0.0345(5) Uani 1 1 d . . . H16A H 0.9373 0.2491 0.3659 0.052 Uiso 1 1 calc R . . H16B H 0.7582 0.2748 0.3190 0.052 Uiso 1 1 calc R . . H16C H 0.7938 0.2116 0.2647 0.052 Uiso 1 1 calc R . . C17 C 0.4429(2) 0.24695(8) 0.34208(19) 0.0254(5) Uani 1 1 d . . . H17 H 0.4606 0.2589 0.2589 0.031 Uiso 1 1 calc R . . C18 C 0.4842(3) 0.30145(9) 0.4333(2) 0.0401(6) Uani 1 1 d . . . H18A H 0.4132 0.3348 0.3913 0.060 Uiso 1 1 calc R . . H18B H 0.5958 0.3131 0.4501 0.060 Uiso 1 1 calc R . . H18C H 0.4700 0.2914 0.5170 0.060 Uiso 1 1 calc R . . C19 C 0.2654(2) 0.23154(9) 0.3045(2) 0.0399(6) Uani 1 1 d . . . H19A H 0.2409 0.2228 0.3844 0.060 Uiso 1 1 calc R . . H19B H 0.2409 0.1963 0.2467 0.060 Uiso 1 1 calc R . . H19C H 0.2006 0.2655 0.2581 0.060 Uiso 1 1 calc R . . C20 C 0.5340(2) 0.14616(9) 0.55194(19) 0.0304(5) Uani 1 1 d . . . H20A H 0.6334 0.1280 0.6132 0.037 Uiso 1 1 calc R . . H20B H 0.4998 0.1777 0.6011 0.037 Uiso 1 1 calc R . . C21 C 0.4024(2) 0.09746(9) 0.50957(19) 0.0309(5) Uani 1 1 d . . . H21A H 0.3083 0.1140 0.4387 0.037 Uiso 1 1 calc R . . H21B H 0.4432 0.0632 0.4721 0.037 Uiso 1 1 calc R . . C22 C 0.3486(3) 0.07466(9) 0.6187(2) 0.0364(5) Uani 1 1 d . . . H22A H 0.3030 0.1084 0.6539 0.044 Uiso 1 1 calc R . . H22B H 0.4429 0.0594 0.6912 0.044 Uiso 1 1 calc R . . C23 C 0.2238(3) 0.02507(9) 0.5741(2) 0.0387(5) Uani 1 1 d . . . H23A H 0.1285 0.0403 0.5043 0.058 Uiso 1 1 calc R . . H23B H 0.1941 0.0117 0.6491 0.058 Uiso 1 1 calc R . . H23C H 0.2685 -0.0087 0.5402 0.058 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 0.0240(3) 0.0217(3) 0.0219(3) -0.0048(2) 0.0106(2) -0.0025(2) C1 0.0180(10) 0.0165(9) 0.0184(9) 0.0012(7) 0.0069(8) 0.0021(7) C2 0.0187(10) 0.0147(9) 0.0199(9) 0.0021(7) 0.0076(8) 0.0027(7) C3 0.0219(10) 0.0171(9) 0.0218(10) -0.0030(8) 0.0078(9) 0.0020(8) C4 0.0185(10) 0.0183(10) 0.0229(10) 0.0021(8) 0.0070(8) 0.0031(8) C5 0.0216(11) 0.0206(10) 0.0312(11) -0.0017(9) 0.0090(9) -0.0012(8) C6 0.0225(11) 0.0253(11) 0.0372(11) 0.0037(9) 0.0111(9) -0.0027(9) C7 0.0227(11) 0.0311(12) 0.0284(11) 0.0069(9) 0.0135(9) 0.0003(9) C8 0.0230(11) 0.0299(11) 0.0206(10) 0.0022(8) 0.0094(9) 0.0019(9) C9 0.0187(10) 0.0192(10) 0.0218(10) 0.0047(8) 0.0070(8) 0.0026(8) C10 0.0200(10) 0.0191(10) 0.0184(9) -0.0002(7) 0.0064(8) 0.0029(8) C11 0.0174(10) 0.0169(9) 0.0182(9) 0.0021(7) 0.0054(8) 0.0031(7) C12 0.0171(10) 0.0210(10) 0.0225(10) 0.0029(8) 0.0082(8) -0.0009(8) C13 0.0208(10) 0.0218(10) 0.0244(10) -0.0001(8) 0.0111(9) -0.0010(8) C14 0.0261(11) 0.0296(11) 0.0268(11) -0.0081(9) 0.0088(9) -0.0035(9) C15 0.0255(12) 0.0520(15) 0.0461(14) 0.0046(12) 0.0055(11) 0.0052(11) C16 0.0273(12) 0.0332(12) 0.0475(14) -0.0037(10) 0.0185(11) -0.0060(10) C17 0.0266(11) 0.0244(11) 0.0276(10) -0.0026(8) 0.0124(9) -0.0016(9) C18 0.0315(13) 0.0291(12) 0.0593(15) -0.0146(11) 0.0152(12) 0.0006(10) C19 0.0248(12) 0.0355(13) 0.0514(14) -0.0063(11) 0.0027(11) 0.0015(10) C20 0.0371(13) 0.0310(12) 0.0265(11) -0.0029(9) 0.0151(10) -0.0015(10) C21 0.0366(13) 0.0309(12) 0.0299(11) 0.0020(9) 0.0174(10) -0.0008(10) C22 0.0353(13) 0.0446(14) 0.0331(12) 0.0102(10) 0.0166(11) 0.0026(11) C23 0.0391(13) 0.0379(13) 0.0449(13) 0.0106(11) 0.0219(11) 0.0016(11) _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 C13 1.8393(19) . ? Si1 C20 1.8702(19) . ? Si1 C17 1.8800(19) . ? Si1 C14 1.881(2) . ? C1 C11 1.415(2) 3_655 ? C1 C12 1.426(2) . ? C1 C2 1.426(2) . ? C2 C3 1.406(2) . ? C2 C11 1.439(2) . ? C3 C4 1.384(2) . ? C3 H3 0.9500 . ? C4 C5 1.423(2) . ? C4 C9 1.442(2) . ? C5 C6 1.353(2) . ? C5 H5 0.9500 . ? C6 C7 1.420(3) . ? C6 H6 0.9500 . ? C7 C8 1.350(2) . ? C7 H7 0.9500 . ? C8 C9 1.441(2) . ? C8 H8 0.9500 . ? C9 C10 1.387(2) . ? C10 C11 1.414(2) . ? C10 H10 0.9500 . ? C11 C1 1.415(2) 3_655 ? C12 C13 1.209(2) . ? C14 C15 1.531(3) . ? C14 C16 1.536(3) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.525(3) . ? C17 C18 1.528(3) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.545(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.505(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.523(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 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 C13 Si1 C20 107.00(9) . . ? C13 Si1 C17 108.06(8) . . ? C20 Si1 C17 111.32(9) . . ? C13 Si1 C14 106.22(8) . . ? C20 Si1 C14 113.95(9) . . ? C17 Si1 C14 109.97(9) . . ? C11 C1 C12 120.43(15) 3_655 . ? C11 C1 C2 120.74(15) 3_655 . ? C12 C1 C2 118.82(16) . . ? C3 C2 C1 121.50(16) . . ? C3 C2 C11 118.98(15) . . ? C1 C2 C11 119.52(15) . . ? C4 C3 C2 122.11(16) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C3 C4 C5 122.04(17) . . ? C3 C4 C9 119.13(16) . . ? C5 C4 C9 118.83(16) . . ? C6 C5 C4 120.97(18) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 120.43(18) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 121.32(18) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C7 C8 C9 120.34(18) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 122.52(17) . . ? C10 C9 C4 119.38(16) . . ? C8 C9 C4 118.10(16) . . ? C9 C10 C11 121.81(16) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C10 C11 C1 121.73(16) . 3_655 ? C10 C11 C2 118.55(16) . . ? C1 C11 C2 119.71(15) 3_655 . ? C13 C12 C1 178.45(19) . . ? C12 C13 Si1 177.44(17) . . ? C15 C14 C16 110.18(16) . . ? C15 C14 Si1 112.14(14) . . ? C16 C14 Si1 111.24(13) . . ? C15 C14 H14 107.7 . . ? C16 C14 H14 107.7 . . ? Si1 C14 H14 107.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 110.36(16) . . ? C19 C17 Si1 113.80(13) . . ? C18 C17 Si1 111.83(14) . . ? C19 C17 H17 106.8 . . ? C18 C17 H17 106.8 . . ? Si1 C17 H17 106.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 Si1 114.77(13) . . ? C21 C20 H20A 108.6 . . ? Si1 C20 H20A 108.6 . . ? C21 C20 H20B 108.6 . . ? Si1 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C22 C21 C20 114.72(17) . . ? C22 C21 H21A 108.6 . . ? C20 C21 H21A 108.6 . . ? C22 C21 H21B 108.6 . . ? C20 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C21 C22 C23 113.05(17) . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C1 C2 C3 -178.67(16) 3_655 . . . ? C12 C1 C2 C3 1.7(2) . . . . ? C11 C1 C2 C11 1.7(3) 3_655 . . . ? C12 C1 C2 C11 -177.94(15) . . . . ? C1 C2 C3 C4 -177.89(16) . . . . ? C11 C2 C3 C4 1.7(3) . . . . ? C2 C3 C4 C5 179.98(17) . . . . ? C2 C3 C4 C9 -0.1(3) . . . . ? C3 C4 C5 C6 -179.88(18) . . . . ? C9 C4 C5 C6 0.2(3) . . . . ? C4 C5 C6 C7 0.3(3) . . . . ? C5 C6 C7 C8 -0.5(3) . . . . ? C6 C7 C8 C9 0.1(3) . . . . ? C7 C8 C9 C10 -178.61(17) . . . . ? C7 C8 C9 C4 0.5(3) . . . . ? C3 C4 C9 C10 -1.4(3) . . . . ? C5 C4 C9 C10 178.49(16) . . . . ? C3 C4 C9 C8 179.49(16) . . . . ? C5 C4 C9 C8 -0.6(2) . . . . ? C8 C9 C10 C11 -179.59(17) . . . . ? C4 C9 C10 C11 1.3(3) . . . . ? C9 C10 C11 C1 179.81(16) . . . 3_655 ? C9 C10 C11 C2 0.2(3) . . . . ? C3 C2 C11 C10 -1.7(2) . . . . ? C1 C2 C11 C10 177.86(16) . . . . ? C3 C2 C11 C1 178.68(16) . . . 3_655 ? C1 C2 C11 C1 -1.7(3) . . . 3_655 ? C13 Si1 C14 C15 -58.71(15) . . . . ? C20 Si1 C14 C15 58.83(16) . . . . ? C17 Si1 C14 C15 -175.39(14) . . . . ? C13 Si1 C14 C16 65.19(15) . . . . ? C20 Si1 C14 C16 -177.28(13) . . . . ? C17 Si1 C14 C16 -51.50(15) . . . . ? C13 Si1 C17 C19 65.22(16) . . . . ? C20 Si1 C17 C19 -52.00(17) . . . . ? C14 Si1 C17 C19 -179.25(14) . . . . ? C13 Si1 C17 C18 -168.89(13) . . . . ? C20 Si1 C17 C18 73.90(15) . . . . ? C14 Si1 C17 C18 -53.36(16) . . . . ? C13 Si1 C20 C21 -31.35(17) . . . . ? C17 Si1 C20 C21 86.50(16) . . . . ? C14 Si1 C20 C21 -148.43(14) . . . . ? Si1 C20 C21 C22 -171.87(15) . . . . ? C20 C21 C22 C23 -177.74(17) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max .358 _refine_diff_density_min -.281 _refine_diff_density_rms .056 # Attachment 'x04048.cif' data_x04048 _database_code_depnum_ccdc_archive 'CCDC 671512' # start Validation Reply Form _vrf_PLAT432_x04048 ; PROBLEM: Short Inter X...Y Contact C21C .. C21D .. 2.82 Ang. RESPONSE: These are both minor occupancy disordered atoms. There is no reason to suggest that there is ever a clash, since their occupancy factors are 0.16, which is well below 0.5. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H50 Si2' _chemical_formula_sum 'C42 H50 Si2' _chemical_formula_weight 611.00 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' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6177(2) _cell_length_b 13.6171(3) _cell_length_c 14.0829(3) _cell_angle_alpha 75.154(1) _cell_angle_beta 73.915(1) _cell_angle_gamma 71.123(1) _cell_volume 1819.86(7) _cell_formula_units_Z 2 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 4638 _cell_measurement_theta_min 4.4 _cell_measurement_theta_max 64.7 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.115 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 1.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9004 _exptl_absorpt_correction_T_max 0.9894 _exptl_absorpt_process_details 'Sadabs in APEX2 (BrukerAXS, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator 'graded multilayer optics' _diffrn_measurement_device_type 'Bruker X8 Proteum diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 18 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 24794 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 67.97 _reflns_number_total 6461 _reflns_number_gt 4402 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker-AXS, 2004)' _computing_cell_refinement 'APEX2 (Bruker-AXS, 2004)' _computing_data_reduction 'APEX2 (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 1994)' _computing_publication_material ; SHELX97-2 (Sheldrick, 1997) and local procedures ; _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^ > 2\s(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^)+(0.1261P)^2^+1.6459P] 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 6461 _refine_ls_number_parameters 416 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2414 _refine_ls_wR_factor_gt 0.2086 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1A Si 0.26486(10) 0.13989(8) 0.23784(7) 0.0459(3) Uani 1 1 d . . . C1A C 0.0618(3) 0.0335(3) 0.0593(3) 0.0396(8) Uani 1 1 d . . . C2A C 0.0920(3) 0.0639(2) -0.0467(3) 0.0390(7) Uani 1 1 d . . . C3A C 0.1813(3) 0.1276(3) -0.0954(3) 0.0425(8) Uani 1 1 d . . . H3A H 0.2225 0.1500 -0.0559 0.051 Uiso 1 1 calc R . . C4A C 0.2108(3) 0.1585(3) -0.1991(3) 0.0449(8) Uani 1 1 d . . . C5A C 0.3020(4) 0.2231(3) -0.2490(3) 0.0537(9) Uani 1 1 d . . . H5A H 0.3453 0.2448 -0.2105 0.064 Uiso 1 1 calc R . . C6A C 0.3270(4) 0.2533(3) -0.3501(3) 0.0613(11) Uani 1 1 d . . . H6A H 0.3872 0.2964 -0.3817 0.074 Uiso 1 1 calc R . . C7A C 0.2641(4) 0.2211(3) -0.4096(3) 0.0605(11) Uani 1 1 d . . . H7A H 0.2822 0.2433 -0.4805 0.073 Uiso 1 1 calc R . . C8A C 0.1789(4) 0.1594(3) -0.3659(3) 0.0533(9) Uani 1 1 d . . . H8A H 0.1381 0.1383 -0.4067 0.064 Uiso 1 1 calc R . . C9A C 0.1492(3) 0.1251(3) -0.2596(3) 0.0436(8) Uani 1 1 d . . . C10A C 0.0616(3) 0.0615(3) -0.2125(3) 0.0427(8) Uani 1 1 d . . . H10A H 0.0216 0.0387 -0.2525 0.051 Uiso 1 1 calc R . . C11A C 0.0307(3) 0.0301(3) -0.1075(3) 0.0399(8) Uani 1 1 d . . . C12A C 0.1243(3) 0.0662(3) 0.1193(3) 0.0412(8) Uani 1 1 d . . . C13A C 0.1776(3) 0.0953(3) 0.1675(3) 0.0443(8) Uani 1 1 d . A . C14A C 0.1921(5) 0.1030(4) 0.3758(3) 0.0654(11) Uani 1 1 d . A . H14A H 0.2354 0.1324 0.4127 0.078 Uiso 1 1 calc R . . C15A C 0.0398(5) 0.1524(4) 0.4028(3) 0.0705(12) Uani 1 1 d . . . H15A H -0.0061 0.1286 0.3649 0.106 Uiso 1 1 calc R A . H15B H 0.0208 0.2295 0.3858 0.106 Uiso 1 1 calc R . . H15C H 0.0063 0.1311 0.4750 0.106 Uiso 1 1 calc R . . C16A C 0.2306(6) -0.0167(4) 0.4106(4) 0.0822(14) Uani 1 1 d . . . H16A H 0.2023 -0.0334 0.4839 0.123 Uiso 1 1 calc R A . H16B H 0.3295 -0.0452 0.3906 0.123 Uiso 1 1 calc R . . H16C H 0.1848 -0.0481 0.3796 0.123 Uiso 1 1 calc R . . C17A C 0.4498(4) 0.0738(3) 0.2019(4) 0.0635(11) Uani 1 1 d . A . H17A H 0.4588 -0.0036 0.2140 0.076 Uiso 1 1 calc R . . C18A C 0.5303(5) 0.0887(5) 0.2699(6) 0.121(3) Uani 1 1 d . . . H18A H 0.6280 0.0616 0.2436 0.181 Uiso 1 1 calc R A . H18B H 0.5053 0.0500 0.3381 0.181 Uiso 1 1 calc R . . H18C H 0.5088 0.1639 0.2715 0.181 Uiso 1 1 calc R . . C19A C 0.5066(5) 0.1060(5) 0.0904(5) 0.101(2) Uani 1 1 d . . . H19A H 0.4886 0.1830 0.0732 0.151 Uiso 1 1 calc R A . H19B H 0.4627 0.0824 0.0510 0.151 Uiso 1 1 calc R . . H19C H 0.6050 0.0734 0.0752 0.151 Uiso 1 1 calc R . . C20A C 0.2238(4) 0.2877(4) 0.2000(4) 0.0714(13) Uani 0.842(7) 1 d PU A 1 H20A H 0.2563 0.3046 0.1262 0.086 Uiso 0.842(7) 1 calc PR A 1 H20B H 0.1234 0.3159 0.2141 0.086 Uiso 0.842(7) 1 calc PR A 1 C21A C 0.2780(7) 0.3447(5) 0.2460(8) 0.140(4) Uani 0.842(7) 1 d PU A 1 H21A H 0.2510 0.3267 0.3194 0.210 Uiso 0.842(7) 1 calc PR A 1 H21B H 0.2420 0.4208 0.2241 0.210 Uiso 0.842(7) 1 calc PR A 1 H21C H 0.3776 0.3251 0.2257 0.210 Uiso 0.842(7) 1 calc PR A 1 C20C C 0.2238(4) 0.2877(4) 0.2000(4) 0.0714(13) Uani 0.158(7) 1 d P A 2 H20C H 0.1249 0.3124 0.2013 0.086 Uiso 0.158(7) 1 calc PR A 2 H20D H 0.2369 0.3135 0.2552 0.086 Uiso 0.158(7) 1 calc PR A 2 C21C C 0.282(2) 0.3403(19) 0.1156(18) 0.053(7) Uiso 0.158(7) 1 d P A 2 H21D H 0.2428 0.4163 0.1140 0.080 Uiso 0.158(7) 1 calc PR A 2 H21E H 0.2672 0.3212 0.0579 0.080 Uiso 0.158(7) 1 calc PR A 2 H21F H 0.3804 0.3222 0.1124 0.080 Uiso 0.158(7) 1 calc PR A 2 Si1B Si 0.72417(10) 0.41587(8) 0.23113(8) 0.0482(3) Uani 1 1 d . . . C1B C 0.9374(3) 0.4814(3) 0.4315(3) 0.0462(8) Uani 1 1 d . . . C2B C 0.9113(3) 0.4327(3) 0.5339(3) 0.0449(8) Uani 1 1 d . . . C3B C 0.8246(4) 0.3662(3) 0.5704(3) 0.0480(9) Uani 1 1 d . . . H3B H 0.7840 0.3527 0.5247 0.058 Uiso 1 1 calc R . . C4B C 0.7963(4) 0.3198(3) 0.6705(3) 0.0482(9) Uani 1 1 d . . . C5B C 0.7059(4) 0.2528(3) 0.7088(3) 0.0535(9) Uani 1 1 d . . . H5B H 0.6637 0.2393 0.6640 0.064 Uiso 1 1 calc R . . C6B C 0.6804(4) 0.2093(3) 0.8062(3) 0.0582(10) Uani 1 1 d . . . H6B H 0.6207 0.1651 0.8295 0.070 Uiso 1 1 calc R . . C7B C 0.7416(4) 0.2283(3) 0.8757(3) 0.0579(10) Uani 1 1 d . . . H7B H 0.7221 0.1970 0.9447 0.070 Uiso 1 1 calc R . . C8B C 0.8272(4) 0.2908(3) 0.8435(3) 0.0554(10) Uani 1 1 d . . . H8B H 0.8674 0.3028 0.8904 0.067 Uiso 1 1 calc R . . C9B C 0.8580(4) 0.3388(3) 0.7407(3) 0.0492(9) Uani 1 1 d . . . C10B C 0.9456(4) 0.4029(3) 0.7051(3) 0.0500(9) Uani 1 1 d . . . H10B H 0.9879 0.4144 0.7510 0.060 Uiso 1 1 calc R . . C11B C 0.9744(3) 0.4515(3) 0.6039(3) 0.0459(8) Uani 1 1 d . . . C12B C 0.8735(4) 0.4631(3) 0.3627(3) 0.0488(9) Uani 1 1 d . . . C13B C 0.8188(4) 0.4452(3) 0.3076(3) 0.0524(9) Uani 1 1 d . A . C14B C 0.8462(4) 0.3225(3) 0.1489(3) 0.0506(9) Uani 1 1 d . A . H14B H 0.9080 0.2692 0.1912 0.061 Uiso 1 1 calc R . . C15B C 0.7777(5) 0.2626(4) 0.1132(3) 0.0695(12) Uani 1 1 d . . . H15D H 0.7107 0.3123 0.0755 0.104 Uiso 1 1 calc R A . H15E H 0.7315 0.2202 0.1713 0.104 Uiso 1 1 calc R . . H15F H 0.8459 0.2160 0.0696 0.104 Uiso 1 1 calc R . . C16B C 0.9376(4) 0.3764(4) 0.0597(3) 0.0694(12) Uani 1 1 d . . . H16D H 1.0093 0.3225 0.0259 0.104 Uiso 1 1 calc R A . H16E H 0.9791 0.4170 0.0843 0.104 Uiso 1 1 calc R . . H16F H 0.8825 0.4239 0.0121 0.104 Uiso 1 1 calc R . . C17B C 0.5919(4) 0.3537(3) 0.3220(3) 0.0578(10) Uani 1 1 d . A . H17B H 0.5417 0.3363 0.2809 0.069 Uiso 1 1 calc R . . C18B C 0.6557(4) 0.2493(4) 0.3869(3) 0.0656(11) Uani 1 1 d . . . H18D H 0.7044 0.2633 0.4296 0.098 Uiso 1 1 calc R A . H18E H 0.7196 0.2009 0.3432 0.098 Uiso 1 1 calc R . . H18F H 0.5837 0.2173 0.4292 0.098 Uiso 1 1 calc R . . C19B C 0.4869(5) 0.4287(4) 0.3881(4) 0.0804(14) Uani 1 1 d . . . H19D H 0.4195 0.3931 0.4328 0.121 Uiso 1 1 calc R A . H19E H 0.4410 0.4917 0.3456 0.121 Uiso 1 1 calc R . . H19F H 0.5326 0.4494 0.4284 0.121 Uiso 1 1 calc R . . C20B C 0.6430(5) 0.5454(3) 0.1560(4) 0.0665(12) Uani 0.842(7) 1 d PU A 1 H20G H 0.5859 0.5938 0.2029 0.080 Uiso 0.842(7) 1 calc PR A 1 H20H H 0.7157 0.5772 0.1122 0.080 Uiso 0.842(7) 1 calc PR A 1 C21B C 0.5548(6) 0.5367(4) 0.0905(5) 0.0774(19) Uani 0.842(7) 1 d PU A 1 H21G H 0.6122 0.4950 0.0391 0.116 Uiso 0.842(7) 1 calc PR A 1 H21H H 0.5106 0.6075 0.0579 0.116 Uiso 0.842(7) 1 calc PR A 1 H21I H 0.4852 0.5021 0.1327 0.116 Uiso 0.842(7) 1 calc PR A 1 C20D C 0.6430(5) 0.5454(3) 0.1560(4) 0.0665(12) Uani 0.158(7) 1 d P A 2 H20E H 0.5901 0.5312 0.1157 0.080 Uiso 0.158(7) 1 calc PR A 2 H20F H 0.5774 0.5898 0.2038 0.080 Uiso 0.158(7) 1 calc PR A 2 C21D C 0.7321(19) 0.6067(15) 0.0887(14) 0.035(5) Uiso 0.158(7) 1 d P A 2 H21J H 0.6774 0.6720 0.0544 0.053 Uiso 0.158(7) 1 calc PR A 2 H21K H 0.7957 0.5655 0.0387 0.053 Uiso 0.158(7) 1 calc PR A 2 H21L H 0.7833 0.6241 0.1273 0.053 Uiso 0.158(7) 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 Si1A 0.0450(6) 0.0541(6) 0.0501(6) -0.0134(4) -0.0119(4) -0.0243(5) C1A 0.0325(16) 0.0389(18) 0.052(2) -0.0135(15) -0.0126(14) -0.0084(14) C2A 0.0326(16) 0.0356(17) 0.051(2) -0.0115(14) -0.0122(14) -0.0072(14) C3A 0.0390(17) 0.0434(19) 0.051(2) -0.0116(15) -0.0120(15) -0.0144(15) C4A 0.0409(18) 0.0432(19) 0.055(2) -0.0119(16) -0.0095(16) -0.0159(15) C5A 0.055(2) 0.059(2) 0.057(2) -0.0106(18) -0.0092(18) -0.0298(19) C6A 0.067(3) 0.067(3) 0.058(2) -0.008(2) -0.003(2) -0.041(2) C7A 0.067(3) 0.074(3) 0.048(2) -0.008(2) -0.0071(19) -0.036(2) C8A 0.054(2) 0.064(2) 0.048(2) -0.0137(18) -0.0086(17) -0.0246(19) C9A 0.0391(18) 0.0459(19) 0.049(2) -0.0127(16) -0.0090(15) -0.0133(15) C10A 0.0376(17) 0.0465(19) 0.049(2) -0.0148(15) -0.0107(15) -0.0114(15) C11A 0.0336(16) 0.0383(17) 0.052(2) -0.0115(15) -0.0134(14) -0.0084(14) C12A 0.0356(17) 0.0446(19) 0.0465(19) -0.0094(15) -0.0075(14) -0.0153(15) C13A 0.0403(18) 0.053(2) 0.0424(19) -0.0085(16) -0.0039(15) -0.0207(16) C14A 0.077(3) 0.075(3) 0.055(2) -0.018(2) -0.018(2) -0.028(2) C15A 0.071(3) 0.090(3) 0.051(2) -0.017(2) -0.002(2) -0.029(3) C16A 0.101(4) 0.080(3) 0.066(3) -0.004(2) -0.019(3) -0.032(3) C17A 0.054(2) 0.056(2) 0.092(3) -0.019(2) -0.023(2) -0.020(2) C18A 0.065(3) 0.098(4) 0.237(8) -0.079(5) -0.077(4) 0.005(3) C19A 0.047(3) 0.096(4) 0.120(5) -0.005(3) 0.017(3) -0.008(3) C20A 0.047(2) 0.063(3) 0.106(4) -0.026(3) -0.002(2) -0.022(2) C21A 0.086(5) 0.068(4) 0.315(13) -0.084(6) -0.108(7) 0.007(3) C20C 0.047(2) 0.063(3) 0.106(4) -0.026(3) -0.002(2) -0.022(2) Si1B 0.0436(5) 0.0558(6) 0.0548(6) -0.0181(5) -0.0199(4) -0.0121(5) C1B 0.0425(19) 0.048(2) 0.056(2) -0.0159(17) -0.0146(16) -0.0133(16) C2B 0.0388(18) 0.0441(19) 0.059(2) -0.0152(16) -0.0161(16) -0.0114(15) C3B 0.0447(19) 0.050(2) 0.059(2) -0.0152(17) -0.0175(17) -0.0153(17) C4B 0.0401(18) 0.046(2) 0.063(2) -0.0168(17) -0.0145(17) -0.0079(16) C5B 0.047(2) 0.053(2) 0.066(3) -0.0161(19) -0.0100(18) -0.0176(18) C6B 0.045(2) 0.053(2) 0.076(3) -0.017(2) -0.0042(19) -0.0161(18) C7B 0.049(2) 0.053(2) 0.062(2) -0.0080(19) -0.0025(18) -0.0113(18) C8B 0.050(2) 0.058(2) 0.056(2) -0.0153(19) -0.0108(18) -0.0086(19) C9B 0.0434(19) 0.049(2) 0.056(2) -0.0130(17) -0.0104(17) -0.0108(17) C10B 0.049(2) 0.054(2) 0.054(2) -0.0155(17) -0.0165(17) -0.0131(17) C11B 0.0419(19) 0.0438(19) 0.058(2) -0.0141(16) -0.0147(16) -0.0116(16) C12B 0.050(2) 0.050(2) 0.055(2) -0.0123(17) -0.0169(17) -0.0172(17) C13B 0.051(2) 0.053(2) 0.060(2) -0.0107(18) -0.0185(18) -0.0172(18) C14B 0.045(2) 0.058(2) 0.053(2) -0.0108(17) -0.0176(17) -0.0128(17) C15B 0.069(3) 0.073(3) 0.068(3) -0.022(2) -0.019(2) -0.012(2) C16B 0.059(3) 0.087(3) 0.066(3) -0.010(2) -0.014(2) -0.027(2) C17B 0.048(2) 0.075(3) 0.062(2) -0.024(2) -0.0155(18) -0.020(2) C18B 0.064(3) 0.083(3) 0.064(3) -0.015(2) -0.017(2) -0.036(2) C19B 0.064(3) 0.091(4) 0.087(3) -0.039(3) 0.002(2) -0.020(3) C20B 0.069(3) 0.061(3) 0.076(3) -0.025(2) -0.032(2) -0.003(2) C21B 0.078(4) 0.061(3) 0.107(4) -0.027(3) -0.069(3) 0.013(3) C20D 0.069(3) 0.061(3) 0.076(3) -0.025(2) -0.032(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1A C13A 1.841(4) . ? Si1A C17A 1.860(4) . ? Si1A C20A 1.881(5) . ? Si1A C14A 1.882(4) . ? C1A C2A 1.417(5) . ? C1A C12A 1.432(5) . ? C1A C11A 1.433(5) 2 ? C2A C3A 1.410(5) . ? C2A C11A 1.439(5) . ? C3A C4A 1.388(5) . ? C3A H3A 0.9500 . ? C4A C9A 1.434(5) . ? C4A C5A 1.436(5) . ? C5A C6A 1.351(6) . ? C5A H5A 0.9500 . ? C6A C7A 1.425(6) . ? C6A H6A 0.9500 . ? C7A C8A 1.349(5) . ? C7A H7A 0.9500 . ? C8A C9A 1.427(5) . ? C8A H8A 0.9500 . ? C9A C10A 1.393(5) . ? C10A C11A 1.406(5) . ? C10A H10A 0.9500 . ? C11A C1A 1.433(5) 2 ? C12A C13A 1.197(5) . ? C14A C15A 1.516(6) . ? C14A C16A 1.528(6) . ? C14A H14A 1.0000 . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C17A C19A 1.521(7) . ? C17A C18A 1.534(6) . ? C17A H17A 1.0000 . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C20A C21A 1.452(7) . ? C20A H20A 0.9900 . ? C20A H20B 0.9900 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C21C H21D 0.9800 . ? C21C H21E 0.9800 . ? C21C H21F 0.9800 . ? Si1B C13B 1.846(4) . ? Si1B C14B 1.869(4) . ? Si1B C20B 1.881(4) . ? Si1B C17B 1.882(4) . ? C1B C2B 1.415(5) . ? C1B C11B 1.423(5) 2_766 ? C1B C12B 1.435(5) . ? C2B C3B 1.404(5) . ? C2B C11B 1.446(5) . ? C3B C4B 1.381(5) . ? C3B H3B 0.9500 . ? C4B C5B 1.439(5) . ? C4B C9B 1.439(5) . ? C5B C6B 1.337(6) . ? C5B H5B 0.9500 . ? C6B C7B 1.426(6) . ? C6B H6B 0.9500 . ? C7B C8B 1.353(6) . ? C7B H7B 0.9500 . ? C8B C9B 1.422(5) . ? C8B H8B 0.9500 . ? C9B C10B 1.386(5) . ? C10B C11B 1.402(5) . ? C10B H10B 0.9500 . ? C11B C1B 1.423(5) 2_766 ? C12B C13B 1.199(5) . ? C14B C15B 1.498(6) . ? C14B C16B 1.539(6) . ? C14B H14B 1.0000 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17B C19B 1.526(6) . ? C17B C18B 1.540(6) . ? C17B H17B 1.0000 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B C21B 1.533(6) . ? C20B H20G 0.9900 . ? C20B H20H 0.9900 . ? C21B H21G 0.9800 . ? C21B H21H 0.9800 . ? C21B H21I 0.9800 . ? C21D H21J 0.9800 . ? C21D H21K 0.9800 . ? C21D H21L 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 C13A Si1A C17A 106.79(17) . . ? C13A Si1A C20A 106.41(19) . . ? C17A Si1A C20A 112.86(19) . . ? C13A Si1A C14A 107.87(18) . . ? C17A Si1A C14A 112.9(2) . . ? C20A Si1A C14A 109.7(2) . . ? C2A C1A C12A 119.8(3) . . ? C2A C1A C11A 120.7(3) . 2 ? C12A C1A C11A 119.4(3) . 2 ? C3A C2A C1A 121.6(3) . . ? C3A C2A C11A 118.4(3) . . ? C1A C2A C11A 120.1(3) . . ? C4A C3A C2A 122.0(3) . . ? C4A C3A H3A 119.0 . . ? C2A C3A H3A 119.0 . . ? C3A C4A C9A 119.5(3) . . ? C3A C4A C5A 122.2(3) . . ? C9A C4A C5A 118.2(3) . . ? C6A C5A C4A 120.8(4) . . ? C6A C5A H5A 119.6 . . ? C4A C5A H5A 119.6 . . ? C5A C6A C7A 120.7(4) . . ? C5A C6A H6A 119.7 . . ? C7A C6A H6A 119.7 . . ? C8A C7A C6A 120.4(4) . . ? C8A C7A H7A 119.8 . . ? C6A C7A H7A 119.8 . . ? C7A C8A C9A 121.1(4) . . ? C7A C8A H8A 119.4 . . ? C9A C8A H8A 119.4 . . ? C10A C9A C8A 122.3(3) . . ? C10A C9A C4A 119.0(3) . . ? C8A C9A C4A 118.7(3) . . ? C9A C10A C11A 121.9(3) . . ? C9A C10A H10A 119.1 . . ? C11A C10A H10A 119.1 . . ? C10A C11A C1A 121.6(3) . 2 ? C10A C11A C2A 119.2(3) . . ? C1A C11A C2A 119.2(3) 2 . ? C13A C12A C1A 178.5(4) . . ? C12A C13A Si1A 177.9(3) . . ? C15A C14A C16A 112.3(4) . . ? C15A C14A Si1A 112.2(3) . . ? C16A C14A Si1A 111.1(3) . . ? C15A C14A H14A 106.9 . . ? C16A C14A H14A 106.9 . . ? Si1A C14A H14A 106.9 . . ? C14A C15A H15A 109.5 . . ? C14A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C14A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C14A C16A H16A 109.5 . . ? C14A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C14A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C19A C17A C18A 113.3(5) . . ? C19A C17A Si1A 111.9(3) . . ? C18A C17A Si1A 111.5(3) . . ? C19A C17A H17A 106.6 . . ? C18A C17A H17A 106.6 . . ? Si1A C17A H17A 106.6 . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C17A C19A H19A 109.5 . . ? C17A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C17A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C21A C20A Si1A 118.3(4) . . ? C21A C20A H20A 107.7 . . ? Si1A C20A H20A 107.7 . . ? C21A C20A H20B 107.7 . . ? Si1A C20A H20B 107.7 . . ? H20A C20A H20B 107.1 . . ? H21D C21C H21E 109.5 . . ? H21D C21C H21F 109.5 . . ? H21E C21C H21F 109.5 . . ? C13B Si1B C14B 108.64(17) . . ? C13B Si1B C20B 106.93(18) . . ? C14B Si1B C20B 112.09(19) . . ? C13B Si1B C17B 106.61(18) . . ? C14B Si1B C17B 110.97(18) . . ? C20B Si1B C17B 111.3(2) . . ? C2B C1B C11B 120.8(3) . 2_766 ? C2B C1B C12B 119.6(3) . . ? C11B C1B C12B 119.6(3) 2_766 . ? C3B C2B C1B 121.7(3) . . ? C3B C2B C11B 118.3(3) . . ? C1B C2B C11B 119.9(3) . . ? C4B C3B C2B 122.4(3) . . ? C4B C3B H3B 118.8 . . ? C2B C3B H3B 118.8 . . ? C3B C4B C5B 122.7(3) . . ? C3B C4B C9B 119.5(3) . . ? C5B C4B C9B 117.8(4) . . ? C6B C5B C4B 121.2(4) . . ? C6B C5B H5B 119.4 . . ? C4B C5B H5B 119.4 . . ? C5B C6B C7B 121.0(4) . . ? C5B C6B H6B 119.5 . . ? C7B C6B H6B 119.5 . . ? C8B C7B C6B 120.2(4) . . ? C8B C7B H7B 119.9 . . ? C6B C7B H7B 119.9 . . ? C7B C8B C9B 121.2(4) . . ? C7B C8B H8B 119.4 . . ? C9B C8B H8B 119.4 . . ? C10B C9B C8B 122.7(3) . . ? C10B C9B C4B 118.6(3) . . ? C8B C9B C4B 118.7(3) . . ? C9B C10B C11B 122.6(3) . . ? C9B C10B H10B 118.7 . . ? C11B C10B H10B 118.7 . . ? C10B C11B C1B 122.2(3) . 2_766 ? C10B C11B C2B 118.6(3) . . ? C1B C11B C2B 119.3(3) 2_766 . ? C13B C12B C1B 177.8(4) . . ? C12B C13B Si1B 175.7(4) . . ? C15B C14B C16B 110.7(3) . . ? C15B C14B Si1B 112.9(3) . . ? C16B C14B Si1B 112.9(3) . . ? C15B C14B H14B 106.6 . . ? C16B C14B H14B 106.6 . . ? Si1B C14B H14B 106.6 . . ? C14B C15B H15D 109.5 . . ? C14B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C14B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C14B C16B H16D 109.5 . . ? C14B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C14B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C19B C17B C18B 110.6(4) . . ? C19B C17B Si1B 112.8(3) . . ? C18B C17B Si1B 112.4(3) . . ? C19B C17B H17B 106.9 . . ? C18B C17B H17B 106.9 . . ? Si1B C17B H17B 106.9 . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17B C19B H19D 109.5 . . ? C17B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C17B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C21B C20B Si1B 114.2(3) . . ? C21B C20B H20G 108.7 . . ? Si1B C20B H20G 108.7 . . ? C21B C20B H20H 108.7 . . ? Si1B C20B H20H 108.7 . . ? H20G C20B H20H 107.6 . . ? H21J C21D H21K 109.5 . . ? H21J C21D H21L 109.5 . . ? H21K C21D H21L 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12A C1A C2A C3A -1.0(5) . . . . ? C11A C1A C2A C3A 179.2(3) 2 . . . ? C12A C1A C2A C11A 179.2(3) . . . . ? C11A C1A C2A C11A -0.6(5) 2 . . . ? C1A C2A C3A C4A -179.5(3) . . . . ? C11A C2A C3A C4A 0.3(5) . . . . ? C2A C3A C4A C9A 0.0(5) . . . . ? C2A C3A C4A C5A -179.8(3) . . . . ? C3A C4A C5A C6A -178.9(4) . . . . ? C9A C4A C5A C6A 1.3(6) . . . . ? C4A C5A C6A C7A -0.4(6) . . . . ? C5A C6A C7A C8A -0.4(7) . . . . ? C6A C7A C8A C9A 0.3(6) . . . . ? C7A C8A C9A C10A 179.9(4) . . . . ? C7A C8A C9A C4A 0.6(6) . . . . ? C3A C4A C9A C10A -0.5(5) . . . . ? C5A C4A C9A C10A 179.3(3) . . . . ? C3A C4A C9A C8A 178.9(3) . . . . ? C5A C4A C9A C8A -1.3(5) . . . . ? C8A C9A C10A C11A -178.6(3) . . . . ? C4A C9A C10A C11A 0.7(5) . . . . ? C9A C10A C11A C1A 178.7(3) . . . 2 ? C9A C10A C11A C2A -0.5(5) . . . . ? C3A C2A C11A C10A 0.0(4) . . . . ? C1A C2A C11A C10A 179.7(3) . . . . ? C3A C2A C11A C1A -179.2(3) . . . 2 ? C1A C2A C11A C1A 0.6(5) . . . 2 ? C13A Si1A C14A C15A -58.9(4) . . . . ? C17A Si1A C14A C15A -176.6(3) . . . . ? C20A Si1A C14A C15A 56.6(4) . . . . ? C13A Si1A C14A C16A 67.8(4) . . . . ? C17A Si1A C14A C16A -49.9(4) . . . . ? C20A Si1A C14A C16A -176.7(3) . . . . ? C13A Si1A C17A C19A 62.4(4) . . . . ? C20A Si1A C17A C19A -54.1(4) . . . . ? C14A Si1A C17A C19A -179.2(3) . . . . ? C13A Si1A C17A C18A -169.5(4) . . . . ? C20A Si1A C17A C18A 73.9(4) . . . . ? C14A Si1A C17A C18A -51.2(4) . . . . ? C13A Si1A C20A C21A 178.8(5) . . . . ? C17A Si1A C20A C21A -64.4(6) . . . . ? C14A Si1A C20A C21A 62.4(6) . . . . ? C11B C1B C2B C3B -180.0(3) 2_766 . . . ? C12B C1B C2B C3B 0.3(5) . . . . ? C11B C1B C2B C11B 0.2(6) 2_766 . . . ? C12B C1B C2B C11B -179.5(3) . . . . ? C1B C2B C3B C4B -178.8(3) . . . . ? C11B C2B C3B C4B 1.0(5) . . . . ? C2B C3B C4B C5B 179.0(3) . . . . ? C2B C3B C4B C9B -0.6(5) . . . . ? C3B C4B C5B C6B -179.8(4) . . . . ? C9B C4B C5B C6B -0.2(5) . . . . ? C4B C5B C6B C7B 0.3(6) . . . . ? C5B C6B C7B C8B -0.2(6) . . . . ? C6B C7B C8B C9B 0.1(6) . . . . ? C7B C8B C9B C10B -179.8(4) . . . . ? C7B C8B C9B C4B 0.0(5) . . . . ? C3B C4B C9B C10B -0.6(5) . . . . ? C5B C4B C9B C10B 179.8(3) . . . . ? C3B C4B C9B C8B 179.7(3) . . . . ? C5B C4B C9B C8B 0.1(5) . . . . ? C8B C9B C10B C11B -179.0(3) . . . . ? C4B C9B C10B C11B 1.2(5) . . . . ? C9B C10B C11B C1B 178.9(3) . . . 2_766 ? C9B C10B C11B C2B -0.8(5) . . . . ? C3B C2B C11B C10B -0.4(5) . . . . ? C1B C2B C11B C10B 179.4(3) . . . . ? C3B C2B C11B C1B 180.0(3) . . . 2_766 ? C1B C2B C11B C1B -0.2(5) . . . 2_766 ? C13B Si1B C14B C15B 158.5(3) . . . . ? C20B Si1B C14B C15B -83.6(3) . . . . ? C17B Si1B C14B C15B 41.6(3) . . . . ? C13B Si1B C14B C16B -74.9(3) . . . . ? C20B Si1B C14B C16B 43.0(3) . . . . ? C17B Si1B C14B C16B 168.2(3) . . . . ? C13B Si1B C17B C19B 64.0(4) . . . . ? C14B Si1B C17B C19B -177.9(3) . . . . ? C20B Si1B C17B C19B -52.3(4) . . . . ? C13B Si1B C17B C18B -61.8(3) . . . . ? C14B Si1B C17B C18B 56.3(3) . . . . ? C20B Si1B C17B C18B -178.1(3) . . . . ? C13B Si1B C20B C21B -177.7(4) . . . . ? C14B Si1B C20B C21B 63.3(4) . . . . ? C17B Si1B C20B C21B -61.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 67.97 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.852 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.072 # Attachment 'x04059.cif' data_x04059 _database_code_depnum_ccdc_archive 'CCDC 671513' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H66 Si2' _chemical_formula_sum 'C50 H66 Si2' _chemical_formula_weight 723.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0181 .0091 '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' Si Si .2541 .3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.3715(2) _cell_length_b 15.4649(2) _cell_length_c 27.5066(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4411.90(12) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 5229 _cell_measurement_theta_min 5.38 _cell_measurement_theta_max 67.57 _exptl_crystal_description 'semi-regular block' _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7360 _exptl_absorpt_correction_T_max 0.9110 _exptl_absorpt_process_details 'Sadabs in APEX2, Bruker-Nonius, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'FR-591 rotating anode' _diffrn_radiation_monochromator 'Montel multilayer optics' _diffrn_measurement_device_type 'Bruker-Nonius X8 Proteum' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 18 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 36054 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 68.19 _reflns_number_total 3995 _reflns_number_gt 3489 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2, Bruker-Nonius, 2004' _computing_cell_refinement 'APEX2, Bruker-Nonius, 2004' _computing_data_reduction 'APEX2, Bruker-Nonius, 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 1994)' _computing_publication_material ; SHELX97-2 (Sheldrick, 1997) and local procedures ; _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^)+(0.0475P)^2^+1.9822P] 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 3995 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.02713(3) 0.67588(2) 0.433901(13) 0.01688(12) Uani 1 1 d . . . C1 C 0.38162(12) 0.53879(8) 0.48579(5) 0.0177(3) Uani 1 1 d . . . C2 C 0.46743(12) 0.50738(8) 0.44969(5) 0.0170(3) Uani 1 1 d . . . C3 C 0.43957(13) 0.51516(8) 0.39982(5) 0.0196(3) Uani 1 1 d . . . H3 H 0.3611 0.5418 0.3902 0.024 Uiso 1 1 calc R . . C4 C 0.52312(13) 0.48506(9) 0.36439(5) 0.0211(3) Uani 1 1 d . . . C5 C 0.49717(16) 0.49484(10) 0.31368(5) 0.0272(3) Uani 1 1 d . . . H5 H 0.4195 0.5220 0.3036 0.033 Uiso 1 1 calc R . . C6 C 0.58153(17) 0.46597(10) 0.27972(6) 0.0329(4) Uani 1 1 d . . . H6 H 0.5635 0.4744 0.2462 0.040 Uiso 1 1 calc R . . C7 C 0.69705(16) 0.42308(10) 0.29398(6) 0.0320(4) Uani 1 1 d . . . H7 H 0.7549 0.4025 0.2698 0.038 Uiso 1 1 calc R . . C8 C 0.72532(14) 0.41131(9) 0.34149(5) 0.0262(3) Uani 1 1 d . . . H8 H 0.8022 0.3818 0.3503 0.031 Uiso 1 1 calc R . . C9 C 0.64105(13) 0.44266(8) 0.37880(5) 0.0209(3) Uani 1 1 d . . . C10 C 0.66984(13) 0.43518(8) 0.42775(5) 0.0197(3) Uani 1 1 d . . . H10 H 0.7478 0.4075 0.4371 0.024 Uiso 1 1 calc R . . C11 C 0.58740(12) 0.46727(8) 0.46421(5) 0.0175(3) Uani 1 1 d . . . C12 C 0.26383(12) 0.57891(8) 0.47086(5) 0.0182(3) Uani 1 1 d . . . C13 C 0.16645(13) 0.61338(9) 0.45657(5) 0.0192(3) Uani 1 1 d . . . C14 C -0.06133(13) 0.71382(9) 0.48971(5) 0.0215(3) Uani 1 1 d . . . H14 H -0.1301 0.7551 0.4792 0.026 Uiso 1 1 calc R . . C15 C 0.02944(14) 0.76178(10) 0.52449(5) 0.0246(3) Uani 1 1 d . . . H15A H -0.0199 0.7839 0.5522 0.037 Uiso 1 1 calc R . . H15B H 0.0702 0.8101 0.5073 0.037 Uiso 1 1 calc R . . H15C H 0.0961 0.7219 0.5362 0.037 Uiso 1 1 calc R . . C16 C -0.12647(16) 0.63759(10) 0.51549(6) 0.0312(4) Uani 1 1 d . . . H16A H -0.0611 0.5949 0.5247 0.047 Uiso 1 1 calc R . . H16B H -0.1892 0.6108 0.4935 0.047 Uiso 1 1 calc R . . H16C H -0.1707 0.6584 0.5447 0.047 Uiso 1 1 calc R . . C17 C -0.07608(13) 0.60300(9) 0.39521(5) 0.0229(3) Uani 1 1 d . . . H17 H -0.1050 0.5537 0.4161 0.028 Uiso 1 1 calc R . . C18 C -0.19695(16) 0.65056(11) 0.37754(7) 0.0367(4) Uani 1 1 d . . . H18A H -0.1715 0.7014 0.3586 0.055 Uiso 1 1 calc R . . H18B H -0.2483 0.6689 0.4056 0.055 Uiso 1 1 calc R . . H18C H -0.2484 0.6118 0.3571 0.055 Uiso 1 1 calc R . . C19 C -0.00112(17) 0.56499(12) 0.35235(6) 0.0396(4) Uani 1 1 d . . . H19A H -0.0568 0.5252 0.3342 0.059 Uiso 1 1 calc R . . H19B H 0.0743 0.5336 0.3645 0.059 Uiso 1 1 calc R . . H19C H 0.0271 0.6118 0.3308 0.059 Uiso 1 1 calc R . . C20 C 0.09422(13) 0.76789(9) 0.39700(5) 0.0212(3) Uani 1 1 d . . . H20A H 0.0298 0.7843 0.3721 0.025 Uiso 1 1 calc R . . H20B H 0.1063 0.8183 0.4187 0.025 Uiso 1 1 calc R . . C21 C 0.22265(13) 0.74887(9) 0.37146(5) 0.0214(3) Uani 1 1 d . . . H21A H 0.2851 0.7275 0.3959 0.026 Uiso 1 1 calc R . . H21B H 0.2090 0.7022 0.3474 0.026 Uiso 1 1 calc R . . C22 C 0.28084(14) 0.82677(9) 0.34560(5) 0.0236(3) Uani 1 1 d . . . H22A H 0.2833 0.8763 0.3684 0.028 Uiso 1 1 calc R . . H22B H 0.2246 0.8430 0.3180 0.028 Uiso 1 1 calc R . . C23 C 0.41700(14) 0.80984(10) 0.32660(6) 0.0268(3) Uani 1 1 d . . . H23A H 0.4507 0.8640 0.3122 0.032 Uiso 1 1 calc R . . H23B H 0.4731 0.7948 0.3545 0.032 Uiso 1 1 calc R . . C24 C 0.42659(16) 0.73871(11) 0.28911(6) 0.0357(4) Uani 1 1 d . . . H24A H 0.3647 0.7505 0.2625 0.043 Uiso 1 1 calc R . . H24B H 0.4020 0.6831 0.3043 0.043 Uiso 1 1 calc R . . C25 C 0.56154(17) 0.73049(12) 0.26780(7) 0.0428(4) Uani 1 1 d . . . H25A H 0.5828 0.7831 0.2497 0.064 Uiso 1 1 calc R . . H25B H 0.5647 0.6806 0.2459 0.064 Uiso 1 1 calc R . . H25C H 0.6240 0.7225 0.2942 0.064 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 0.0135(2) 0.0170(2) 0.0201(2) 0.00127(14) -0.00084(13) 0.00171(13) C1 0.0146(6) 0.0131(6) 0.0254(7) 0.0019(5) -0.0003(5) -0.0007(5) C2 0.0155(6) 0.0124(6) 0.0232(7) 0.0012(5) -0.0006(5) -0.0016(5) C3 0.0185(6) 0.0160(6) 0.0242(7) 0.0012(5) -0.0031(5) 0.0000(5) C4 0.0247(7) 0.0150(6) 0.0235(7) -0.0003(6) -0.0009(6) -0.0020(5) C5 0.0354(8) 0.0224(7) 0.0239(8) -0.0013(6) -0.0043(6) 0.0023(6) C6 0.0483(10) 0.0302(8) 0.0203(7) -0.0030(6) -0.0004(7) 0.0014(7) C7 0.0408(9) 0.0291(8) 0.0261(8) -0.0056(6) 0.0084(7) 0.0017(7) C8 0.0268(7) 0.0225(7) 0.0294(8) -0.0026(6) 0.0050(6) 0.0010(6) C9 0.0218(7) 0.0158(6) 0.0250(7) 0.0004(5) 0.0024(6) -0.0025(5) C10 0.0165(6) 0.0160(6) 0.0265(7) 0.0016(5) 0.0017(5) -0.0002(5) C11 0.0156(6) 0.0130(6) 0.0240(7) 0.0017(5) -0.0001(5) -0.0017(5) C12 0.0172(7) 0.0169(6) 0.0206(7) 0.0008(5) 0.0016(5) -0.0014(5) C13 0.0176(7) 0.0191(6) 0.0209(7) 0.0011(5) 0.0019(5) 0.0002(5) C14 0.0178(6) 0.0212(7) 0.0255(7) 0.0009(6) 0.0017(6) 0.0034(5) C15 0.0244(7) 0.0251(7) 0.0243(7) -0.0030(6) 0.0020(6) 0.0030(6) C16 0.0309(8) 0.0314(8) 0.0312(8) -0.0015(7) 0.0109(7) -0.0052(7) C17 0.0206(7) 0.0211(7) 0.0271(7) 0.0010(6) -0.0012(6) -0.0020(5) C18 0.0308(8) 0.0306(8) 0.0487(10) 0.0004(8) -0.0184(8) -0.0018(7) C19 0.0364(9) 0.0435(10) 0.0388(10) -0.0181(8) 0.0042(7) -0.0118(8) C20 0.0197(7) 0.0211(7) 0.0227(7) 0.0022(6) -0.0018(5) 0.0014(5) C21 0.0200(7) 0.0219(7) 0.0223(7) 0.0019(6) 0.0001(5) -0.0011(5) C22 0.0263(8) 0.0235(7) 0.0211(7) 0.0036(6) -0.0013(6) -0.0017(6) C23 0.0249(8) 0.0293(8) 0.0261(7) 0.0070(6) -0.0004(6) -0.0062(6) C24 0.0307(8) 0.0351(9) 0.0413(10) -0.0011(7) 0.0070(7) -0.0048(7) C25 0.0367(9) 0.0468(10) 0.0450(10) -0.0033(8) 0.0120(8) -0.0026(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 C13 1.8469(14) . ? Si1 C20 1.8812(14) . ? Si1 C14 1.8823(14) . ? Si1 C17 1.8838(14) . ? C1 C11 1.4155(19) 5_666 ? C1 C2 1.4191(19) . ? C1 C12 1.4303(18) . ? C2 C3 1.407(2) . ? C2 C11 1.4465(18) . ? C3 C4 1.385(2) . ? C3 H3 0.9500 . ? C4 C5 1.429(2) . ? C4 C9 1.443(2) . ? C5 C6 1.356(2) . ? C5 H5 0.9500 . ? C6 C7 1.424(2) . ? C6 H6 0.9500 . ? C7 C8 1.352(2) . ? C7 H7 0.9500 . ? C8 C9 1.433(2) . ? C8 H8 0.9500 . ? C9 C10 1.384(2) . ? C10 C11 1.4082(19) . ? C10 H10 0.9500 . ? C11 C1 1.4156(19) 5_666 ? C12 C13 1.2078(19) . ? C14 C16 1.533(2) . ? C14 C15 1.533(2) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.530(2) . ? C17 C18 1.532(2) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.5345(19) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.5237(19) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.528(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.511(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.523(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 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 C13 Si1 C20 106.78(6) . . ? C13 Si1 C14 105.61(6) . . ? C20 Si1 C14 112.61(6) . . ? C13 Si1 C17 108.80(6) . . ? C20 Si1 C17 110.97(6) . . ? C14 Si1 C17 111.73(6) . . ? C11 C1 C2 120.98(12) 5_666 . ? C11 C1 C12 120.10(12) 5_666 . ? C2 C1 C12 118.90(12) . . ? C3 C2 C1 121.61(12) . . ? C3 C2 C11 118.85(12) . . ? C1 C2 C11 119.54(12) . . ? C4 C3 C2 121.93(13) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 122.26(13) . . ? C3 C4 C9 119.33(13) . . ? C5 C4 C9 118.41(13) . . ? C6 C5 C4 121.09(14) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 120.43(14) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 120.76(14) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 120.97(14) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 122.47(13) . . ? C10 C9 C4 119.21(13) . . ? C8 C9 C4 118.31(13) . . ? C9 C10 C11 122.16(13) . . ? C9 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C10 C11 C1 122.05(12) . 5_666 ? C10 C11 C2 118.48(12) . . ? C1 C11 C2 119.47(12) 5_666 . ? C13 C12 C1 177.53(14) . . ? C12 C13 Si1 174.33(12) . . ? C16 C14 C15 110.74(12) . . ? C16 C14 Si1 110.63(10) . . ? C15 C14 Si1 111.12(9) . . ? C16 C14 H14 108.1 . . ? C15 C14 H14 108.1 . . ? Si1 C14 H14 108.1 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 110.84(14) . . ? C19 C17 Si1 112.12(10) . . ? C18 C17 Si1 110.91(10) . . ? C19 C17 H17 107.6 . . ? C18 C17 H17 107.6 . . ? Si1 C17 H17 107.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 Si1 115.03(9) . . ? C21 C20 H20A 108.5 . . ? Si1 C20 H20A 108.5 . . ? C21 C20 H20B 108.5 . . ? Si1 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? C22 C21 C20 113.95(12) . . ? C22 C21 H21A 108.8 . . ? C20 C21 H21A 108.8 . . ? C22 C21 H21B 108.8 . . ? C20 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C21 C22 C23 112.96(12) . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C24 C23 C22 114.76(12) . . ? C24 C23 H23A 108.6 . . ? C22 C23 H23A 108.6 . . ? C24 C23 H23B 108.6 . . ? C22 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? C23 C24 C25 112.57(14) . . ? C23 C24 H24A 109.1 . . ? C25 C24 H24A 109.1 . . ? C23 C24 H24B 109.1 . . ? C25 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C1 C2 C3 -178.19(12) 5_666 . . . ? C12 C1 C2 C3 0.29(19) . . . . ? C11 C1 C2 C11 1.0(2) 5_666 . . . ? C12 C1 C2 C11 179.51(11) . . . . ? C1 C2 C3 C4 179.67(12) . . . . ? C11 C2 C3 C4 0.44(19) . . . . ? C2 C3 C4 C5 -178.24(13) . . . . ? C2 C3 C4 C9 1.4(2) . . . . ? C3 C4 C5 C6 178.97(14) . . . . ? C9 C4 C5 C6 -0.7(2) . . . . ? C4 C5 C6 C7 1.6(2) . . . . ? C5 C6 C7 C8 -0.8(2) . . . . ? C6 C7 C8 C9 -0.9(2) . . . . ? C7 C8 C9 C10 -177.02(14) . . . . ? C7 C8 C9 C4 1.7(2) . . . . ? C3 C4 C9 C10 -1.82(19) . . . . ? C5 C4 C9 C10 177.87(13) . . . . ? C3 C4 C9 C8 179.38(12) . . . . ? C5 C4 C9 C8 -0.94(19) . . . . ? C8 C9 C10 C11 179.07(13) . . . . ? C4 C9 C10 C11 0.3(2) . . . . ? C9 C10 C11 C1 -178.60(12) . . . 5_666 ? C9 C10 C11 C2 1.54(19) . . . . ? C3 C2 C11 C10 -1.91(18) . . . . ? C1 C2 C11 C10 178.84(12) . . . . ? C3 C2 C11 C1 178.23(12) . . . 5_666 ? C1 C2 C11 C1 -1.0(2) . . . 5_666 ? C13 Si1 C14 C16 -69.97(11) . . . . ? C20 Si1 C14 C16 173.86(10) . . . . ? C17 Si1 C14 C16 48.17(12) . . . . ? C13 Si1 C14 C15 53.47(11) . . . . ? C20 Si1 C14 C15 -62.71(11) . . . . ? C17 Si1 C14 C15 171.60(9) . . . . ? C13 Si1 C17 C19 -58.38(13) . . . . ? C20 Si1 C17 C19 58.82(13) . . . . ? C14 Si1 C17 C19 -174.59(11) . . . . ? C13 Si1 C17 C18 177.13(11) . . . . ? C20 Si1 C17 C18 -65.68(12) . . . . ? C14 Si1 C17 C18 60.91(13) . . . . ? C13 Si1 C20 C21 30.56(12) . . . . ? C14 Si1 C20 C21 146.03(10) . . . . ? C17 Si1 C20 C21 -87.87(11) . . . . ? Si1 C20 C21 C22 -174.81(10) . . . . ? C20 C21 C22 C23 171.93(12) . . . . ? C21 C22 C23 C24 61.85(17) . . . . ? C22 C23 C24 C25 174.36(14) . . . . ? _diffrn_measured_fraction_theta_max .989 _diffrn_reflns_theta_full 68.19 _diffrn_measured_fraction_theta_full .989 _refine_diff_density_max .291 _refine_diff_density_min -.246 _refine_diff_density_rms .041