# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email anthony@uky.edu _publ_contact_author_name 'Anthony, John E.' loop_ _publ_author_name 'Zhong Li' 'Yee-Fun Lim' 'Jongbok Kim' 'Sean Parkin' 'Lynn Loo' 'George Malliaras' 'John E.Anthony' data_x10193t4 _database_code_depnum_ccdc_archive 'CCDC 824023' #TrackingRef '- anti_ADTA.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H52 N2 O2 S2 Si2' _chemical_formula_sum 'C44 H52 N2 O2 S2 Si2' _chemical_formula_weight 761.18 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 10.6703(3) _cell_length_b 16.2068(4) _cell_length_c 12.0490(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.683(1) _cell_angle_gamma 90.00 _cell_volume 1995.94(9) _cell_formula_units_Z 2 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 9289 _cell_measurement_theta_min 4.33 _cell_measurement_theta_max 68.44 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 2.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.791 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details 'Sadabs in APEX2 (BrukerAXS, 2006)' _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 5.6 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 47559 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.33 _diffrn_reflns_theta_max 68.59 _reflns_number_total 3647 _reflns_number_gt 3522 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 2008)' _computing_publication_material ; SHELX-97 (Sheldrick, 2008) and local procedures ; _publ_section_exptl_refinement ; H atoms were found in difference Fourier maps and subsequently placed in idealized positions with constrained distances of 0.98 \%A (RCH~3~), 0.99 \%A (R~2~CH~2~), 0.95 \%A (C~Ar~H), and with U~iso~(H) values set to either 1.2U~eq~ or 1.5U~eq~ (RCH~3~, OH) of the attached atom. To ensure stable refinement, the disordered components were subject to constraints (SHELXL97 commands EXYZ and EADP) and restraints (SHELXL97 command SAME). ; _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^)+(0.0749P)^2^+1.9380P] 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 3647 _refine_ls_number_parameters 248 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1445 _refine_ls_wR_factor_gt 0.1390 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.189 _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 Si1 Si 0.72579(6) -0.03384(4) 0.11129(5) 0.01876(19) Uani 1 1 d . . . O1 O -0.06008(17) 0.28818(11) 0.09092(14) 0.0270(4) Uani 1 1 d . B . N1 N -0.17721(19) 0.26275(12) 0.21624(17) 0.0221(4) Uani 1 1 d . B . C1 C 0.5473(2) -0.00309(13) 0.40195(19) 0.0181(5) Uani 1 1 d . . . C2 C 0.4320(2) 0.04182(13) 0.39589(19) 0.0177(5) Uani 1 1 d . B . C3 C 0.3622(2) 0.08289(14) 0.29314(19) 0.0195(5) Uani 1 1 d . . . H3 H 0.3930 0.0809 0.2266 0.023 Uiso 1 1 calc R A 1 C4 C 0.2503(2) 0.12547(14) 0.28966(19) 0.0197(5) Uani 0.905(3) 1 d PD B 1 S5 S 0.15107(6) 0.17926(4) 0.17050(6) 0.0194(2) Uani 0.905(3) 1 d PD B 1 C6 C 0.0430(9) 0.2054(8) 0.2516(4) 0.0184(7) Uani 0.905(3) 1 d PD B 1 C7 C 0.0837(4) 0.1779(3) 0.3617(4) 0.0191(7) Uani 0.905(3) 1 d PD B 1 H7 H 0.0374 0.1888 0.4167 0.023 Uiso 0.905(3) 1 calc PR B 1 C8 C 0.2029(2) 0.13092(13) 0.3892(2) 0.0198(5) Uani 0.905(3) 1 d PD B 1 C4' C 0.2503(2) 0.12547(14) 0.28966(19) 0.0197(5) Uani 0.095(3) 1 d PD B 2 C5' C 0.147(2) 0.166(2) 0.2032(17) 0.0194(2) Uani 0.095(3) 1 d PD B 2 H5' H 0.1442 0.1652 0.1236 0.023 Uiso 0.095(3) 1 calc PR B 2 C6' C 0.054(9) 0.204(8) 0.241(4) 0.0184(7) Uani 0.095(3) 1 d PD B 2 S7' S 0.0685(11) 0.1881(7) 0.3914(10) 0.0191(7) Uani 0.095(3) 1 d PD B 2 C8' C 0.2029(2) 0.13092(13) 0.3892(2) 0.0198(5) Uani 0.095(3) 1 d PD B 2 C9 C 0.2686(2) 0.09168(14) 0.48962(19) 0.0192(5) Uani 1 1 d . . . H9 H 0.2368 0.0953 0.5555 0.023 Uiso 1 1 calc R B 1 C10 C 0.3839(2) 0.04550(13) 0.49662(19) 0.0177(5) Uani 1 1 d . . . C11 C 0.5963(2) -0.00695(13) 0.30308(19) 0.0194(5) Uani 1 1 d . . . C12 C 0.6413(2) -0.01241(14) 0.22204(19) 0.0202(5) Uani 1 1 d . . . C13 C 0.8877(2) -0.07871(14) 0.1908(2) 0.0233(5) Uani 1 1 d . . . H13A H 0.8726 -0.1280 0.2338 0.028 Uiso 1 1 calc R . . H13B H 0.9321 -0.0973 0.1335 0.028 Uiso 1 1 calc R . . C14 C 0.9788(3) -0.02039(17) 0.2759(2) 0.0334(6) Uani 1 1 d . . . H14A H 1.0017 0.0261 0.2335 0.050 Uiso 1 1 calc R . . H14B H 1.0585 -0.0500 0.3176 0.050 Uiso 1 1 calc R . . H14C H 0.9347 0.0003 0.3313 0.050 Uiso 1 1 calc R . . C15 C 0.6281(2) -0.11402(16) 0.0118(2) 0.0243(5) Uani 1 1 d . . . H15A H 0.5465 -0.0886 -0.0370 0.029 Uiso 1 1 calc R . . H15B H 0.6787 -0.1337 -0.0403 0.029 Uiso 1 1 calc R . . C16 C 0.5930(3) -0.18796(16) 0.0759(2) 0.0296(6) Uani 1 1 d . . . H16A H 0.6728 -0.2108 0.1292 0.044 Uiso 1 1 calc R . . H16B H 0.5502 -0.2303 0.0197 0.044 Uiso 1 1 calc R . . H16C H 0.5334 -0.1702 0.1198 0.044 Uiso 1 1 calc R . . C17 C 0.7406(3) 0.06445(15) 0.0334(2) 0.0283(6) Uani 1 1 d . . . H17A H 0.6529 0.0799 -0.0170 0.034 Uiso 1 1 calc R . . H17B H 0.7702 0.1089 0.0914 0.034 Uiso 1 1 calc R . . C18 C 0.8345(2) 0.05943(15) -0.0403(2) 0.0262(5) Uani 1 1 d . . . H18A H 0.9230 0.0481 0.0096 0.039 Uiso 1 1 calc R . . H18B H 0.8341 0.1120 -0.0806 0.039 Uiso 1 1 calc R . . H18C H 0.8070 0.0150 -0.0973 0.039 Uiso 1 1 calc R . . C19 C -0.0689(2) 0.25537(14) 0.18143(19) 0.0208(5) Uani 1 1 d . . . C20 C -0.2880(2) 0.31133(16) 0.1440(2) 0.0284(6) Uani 1 1 d . . . H20A H -0.3210 0.2875 0.0654 0.034 Uiso 1 1 calc R B . H20B H -0.2623 0.3694 0.1376 0.034 Uiso 1 1 calc R . . C21 C -0.3899(2) 0.30485(16) 0.2099(2) 0.0288(6) Uani 1 1 d . B . H21A H -0.3775 0.3486 0.2694 0.035 Uiso 1 1 calc R . . H21B H -0.4797 0.3087 0.1567 0.035 Uiso 1 1 calc R . . C22 C -0.3641(2) 0.21984(16) 0.2655(2) 0.0262(5) Uani 1 1 d . . . H22A H -0.4024 0.1759 0.2087 0.031 Uiso 1 1 calc R B . H22B H -0.4007 0.2153 0.3321 0.031 Uiso 1 1 calc R . . C23 C -0.2149(2) 0.21430(15) 0.3051(2) 0.0230(5) Uani 1 1 d . B . H23A H -0.1785 0.2387 0.3831 0.028 Uiso 1 1 calc R . . H23B H -0.1850 0.1564 0.3063 0.028 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 0.0198(3) 0.0211(3) 0.0176(3) 0.0018(2) 0.0088(3) 0.0026(2) O1 0.0264(9) 0.0317(9) 0.0201(9) 0.0058(7) 0.0020(7) -0.0009(7) N1 0.0198(10) 0.0225(10) 0.0217(10) 0.0030(8) 0.0022(8) 0.0023(8) C1 0.0207(11) 0.0183(10) 0.0158(11) -0.0016(8) 0.0061(9) -0.0014(9) C2 0.0174(11) 0.0180(10) 0.0176(11) -0.0017(8) 0.0047(9) -0.0027(8) C3 0.0206(11) 0.0217(11) 0.0159(11) -0.0010(8) 0.0049(9) -0.0014(9) C4 0.0209(11) 0.0191(10) 0.0172(11) -0.0011(8) 0.0025(9) -0.0013(9) S5 0.0201(3) 0.0236(4) 0.0150(4) 0.0027(2) 0.0058(3) 0.0033(2) C6 0.021(2) 0.0191(11) 0.0175(14) -0.0006(17) 0.0082(11) -0.0008(15) C7 0.0156(14) 0.0208(15) 0.022(2) -0.0020(14) 0.0077(13) 0.0036(10) C8 0.0176(11) 0.0184(10) 0.0240(12) -0.0016(9) 0.0067(9) -0.0011(8) C4' 0.0209(11) 0.0191(10) 0.0172(11) -0.0011(8) 0.0025(9) -0.0013(9) C5' 0.0201(3) 0.0236(4) 0.0150(4) 0.0027(2) 0.0058(3) 0.0033(2) C6' 0.021(2) 0.0191(11) 0.0175(14) -0.0006(17) 0.0082(11) -0.0008(15) S7' 0.0156(14) 0.0208(15) 0.022(2) -0.0020(14) 0.0077(13) 0.0036(10) C8' 0.0176(11) 0.0184(10) 0.0240(12) -0.0016(9) 0.0067(9) -0.0011(8) C9 0.0188(11) 0.0222(11) 0.0194(11) -0.0021(9) 0.0097(9) -0.0012(9) C10 0.0178(11) 0.0187(10) 0.0169(11) -0.0011(8) 0.0058(9) -0.0009(8) C11 0.0188(11) 0.0184(11) 0.0211(12) 0.0023(8) 0.0056(9) 0.0027(8) C12 0.0211(11) 0.0231(11) 0.0180(11) 0.0023(9) 0.0083(9) 0.0033(9) C13 0.0204(12) 0.0223(11) 0.0270(12) 0.0004(9) 0.0063(10) 0.0011(9) C14 0.0317(14) 0.0283(13) 0.0354(15) -0.0002(11) 0.0018(11) -0.0008(11) C15 0.0215(12) 0.0342(13) 0.0177(11) -0.0010(9) 0.0064(9) 0.0014(9) C16 0.0272(13) 0.0282(13) 0.0303(13) -0.0025(10) 0.0035(11) -0.0026(10) C17 0.0325(13) 0.0259(12) 0.0309(13) 0.0079(10) 0.0165(11) 0.0089(10) C18 0.0287(13) 0.0283(12) 0.0256(13) 0.0049(10) 0.0141(10) 0.0012(10) C19 0.0215(11) 0.0205(11) 0.0175(11) 0.0003(8) 0.0008(9) -0.0023(9) C20 0.0216(12) 0.0277(12) 0.0315(13) 0.0049(10) 0.0006(10) 0.0041(10) C21 0.0220(12) 0.0282(12) 0.0325(14) -0.0039(10) 0.0016(10) 0.0044(10) C22 0.0218(12) 0.0307(13) 0.0269(13) -0.0027(10) 0.0085(10) 0.0008(10) C23 0.0220(12) 0.0250(12) 0.0227(12) 0.0006(9) 0.0075(9) 0.0011(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 Si1 C12 1.845(2) . ? Si1 C13 1.866(2) . ? Si1 C15 1.870(2) . ? Si1 C17 1.878(2) . ? O1 C19 1.241(3) . ? N1 C19 1.343(3) . ? N1 C23 1.474(3) . ? N1 C20 1.478(3) . ? C1 C10 1.411(3) 3_656 ? C1 C2 1.413(3) . ? C1 C11 1.434(3) . ? C2 C3 1.415(3) . ? C2 C10 1.448(3) . ? C3 C4 1.369(3) . ? C3 H3 0.9500 . ? C4 C8 1.433(3) . ? C4 S5 1.752(2) . ? S5 C6 1.763(3) . ? C6 C7 1.348(5) . ? C6 C19 1.489(4) . ? C7 C8 1.437(5) . ? C7 H7 0.9500 . ? C8 C9 1.368(3) . ? C5' C6' 1.360(19) . ? C5' H5' 0.9500 . ? C6' C19 1.55(2) . ? C6' S7' 1.79(2) . ? C9 C10 1.422(3) . ? C9 H9 0.9500 . ? C10 C1 1.411(3) 3_656 ? C11 C12 1.208(3) . ? C13 C14 1.522(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.530(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.520(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C20 C21 1.523(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.522(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.528(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? 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 C12 Si1 C13 105.93(11) . . ? C12 Si1 C15 107.25(11) . . ? C13 Si1 C15 108.79(11) . . ? C12 Si1 C17 109.29(11) . . ? C13 Si1 C17 112.89(11) . . ? C15 Si1 C17 112.35(12) . . ? C19 N1 C23 128.17(19) . . ? C19 N1 C20 118.5(2) . . ? C23 N1 C20 111.90(19) . . ? C10 C1 C2 121.6(2) 3_656 . ? C10 C1 C11 118.4(2) 3_656 . ? C2 C1 C11 120.0(2) . . ? C1 C2 C3 121.3(2) . . ? C1 C2 C10 119.4(2) . . ? C3 C2 C10 119.4(2) . . ? C4 C3 C2 119.9(2) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C8 121.3(2) . . ? C3 C4 S5 126.34(18) . . ? C8 C4 S5 112.31(17) . . ? C4 S5 C6 90.20(13) . . ? C7 C6 C19 135.8(3) . . ? C7 C6 S5 112.9(3) . . ? C19 C6 S5 111.2(2) . . ? C6 C7 C8 114.6(3) . . ? C6 C7 H7 122.7 . . ? C8 C7 H7 122.7 . . ? C9 C8 C4 119.8(2) . . ? C9 C8 C7 130.2(3) . . ? C4 C8 C7 110.0(2) . . ? C6' C5' H5' 121.8 . . ? C5' C6' C19 134.0(19) . . ? C5' C6' S7' 114.5(16) . . ? C19 C6' S7' 111.4(15) . . ? C8 C9 C10 120.8(2) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C1 C10 C9 122.3(2) 3_656 . ? C1 C10 C2 119.0(2) 3_656 . ? C9 C10 C2 118.7(2) . . ? C12 C11 C1 177.4(2) . . ? C11 C12 Si1 171.1(2) . . ? C14 C13 Si1 114.94(17) . . ? C14 C13 H13A 108.5 . . ? Si1 C13 H13A 108.5 . . ? C14 C13 H13B 108.5 . . ? Si1 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 Si1 113.13(16) . . ? C16 C15 H15A 109.0 . . ? Si1 C15 H15A 109.0 . . ? C16 C15 H15B 109.0 . . ? Si1 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 Si1 114.24(17) . . ? C18 C17 H17A 108.7 . . ? Si1 C17 H17A 108.7 . . ? C18 C17 H17B 108.7 . . ? Si1 C17 H17B 108.7 . . ? H17A C17 H17B 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 . . ? O1 C19 N1 121.7(2) . . ? O1 C19 C6 118.7(3) . . ? N1 C19 C6 119.6(3) . . ? O1 C19 C6' 112(2) . . ? N1 C19 C6' 126(3) . . ? N1 C20 C21 103.1(2) . . ? N1 C20 H20A 111.1 . . ? C21 C20 H20A 111.1 . . ? N1 C20 H20B 111.1 . . ? C21 C20 H20B 111.1 . . ? H20A C20 H20B 109.1 . . ? C22 C21 C20 103.05(19) . . ? C22 C21 H21A 111.2 . . ? C20 C21 H21A 111.2 . . ? C22 C21 H21B 111.2 . . ? C20 C21 H21B 111.2 . . ? H21A C21 H21B 109.1 . . ? C21 C22 C23 103.4(2) . . ? C21 C22 H22A 111.1 . . ? C23 C22 H22A 111.1 . . ? C21 C22 H22B 111.1 . . ? C23 C22 H22B 111.1 . . ? H22A C22 H22B 109.1 . . ? N1 C23 C22 102.63(19) . . ? N1 C23 H23A 111.2 . . ? C22 C23 H23A 111.2 . . ? N1 C23 H23B 111.2 . . ? C22 C23 H23B 111.2 . . ? H23A C23 H23B 109.2 . . ? 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 C10 C1 C2 C3 -178.8(2) 3_656 . . . ? C11 C1 C2 C3 0.6(3) . . . . ? C10 C1 C2 C10 0.9(3) 3_656 . . . ? C11 C1 C2 C10 -179.7(2) . . . . ? C1 C2 C3 C4 179.6(2) . . . . ? C10 C2 C3 C4 -0.1(3) . . . . ? C2 C3 C4 C8 1.2(3) . . . . ? C2 C3 C4 S5 -179.60(17) . . . . ? C3 C4 S5 C6 178.6(5) . . . . ? C8 C4 S5 C6 -2.2(5) . . . . ? C4 S5 C6 C7 2.5(9) . . . . ? C4 S5 C6 C19 -179.5(8) . . . . ? C19 C6 C7 C8 -179.4(12) . . . . ? S5 C6 C7 C8 -2.1(12) . . . . ? C3 C4 C8 C9 -1.3(3) . . . . ? S5 C4 C8 C9 179.45(17) . . . . ? C3 C4 C8 C7 -179.3(3) . . . . ? S5 C4 C8 C7 1.5(3) . . . . ? C6 C7 C8 C9 -177.3(8) . . . . ? C6 C7 C8 C4 0.4(8) . . . . ? C4 C8 C9 C10 0.1(3) . . . . ? C7 C8 C9 C10 177.6(3) . . . . ? C8 C9 C10 C1 -178.8(2) . . . 3_656 ? C8 C9 C10 C2 1.0(3) . . . . ? C1 C2 C10 C1 -0.8(3) . . . 3_656 ? C3 C2 C10 C1 178.8(2) . . . 3_656 ? C1 C2 C10 C9 179.3(2) . . . . ? C3 C2 C10 C9 -1.0(3) . . . . ? C12 Si1 C13 C14 -64.9(2) . . . . ? C15 Si1 C13 C14 -179.95(18) . . . . ? C17 Si1 C13 C14 54.6(2) . . . . ? C12 Si1 C15 C16 -49.0(2) . . . . ? C13 Si1 C15 C16 65.1(2) . . . . ? C17 Si1 C15 C16 -169.14(17) . . . . ? C12 Si1 C17 C18 166.78(18) . . . . ? C13 Si1 C17 C18 49.2(2) . . . . ? C15 Si1 C17 C18 -74.3(2) . . . . ? C23 N1 C19 O1 165.5(2) . . . . ? C20 N1 C19 O1 0.0(3) . . . . ? C23 N1 C19 C6 -13.4(7) . . . . ? C20 N1 C19 C6 -178.9(7) . . . . ? C23 N1 C19 C6' -12(7) . . . . ? C20 N1 C19 C6' -177(7) . . . . ? C7 C6 C19 O1 161.0(13) . . . . ? S5 C6 C19 O1 -16.3(11) . . . . ? C7 C6 C19 N1 -20.1(19) . . . . ? S5 C6 C19 N1 162.6(5) . . . . ? C5' C6' C19 O1 -26(18) . . . . ? S7' C6' C19 O1 159(6) . . . . ? C5' C6' C19 N1 152(11) . . . . ? S7' C6' C19 N1 -23(12) . . . . ? C19 N1 C20 C21 179.6(2) . . . . ? C23 N1 C20 C21 11.9(3) . . . . ? N1 C20 C21 C22 -31.9(2) . . . . ? C20 C21 C22 C23 40.5(2) . . . . ? C19 N1 C23 C22 -153.3(2) . . . . ? C20 N1 C23 C22 12.9(3) . . . . ? C21 C22 C23 N1 -32.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 68.59 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.593 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.078 # Attachment '- syn_ADTA.cif' data_x10148 _database_code_depnum_ccdc_archive 'CCDC 824024' #TrackingRef '- syn_ADTA.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H52 N2 O2 S2 Si2, C7 H8' _chemical_formula_sum 'C51 H60 N2 O2 S2 Si2' _chemical_formula_weight 853.31 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 11.1843(3) _cell_length_b 14.8367(4) _cell_length_c 15.7732(4) _cell_angle_alpha 63.054(1) _cell_angle_beta 77.064(1) _cell_angle_gamma 89.140(1) _cell_volume 2262.72(10) _cell_formula_units_Z 2 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 9786 _cell_measurement_theta_min 3.43 _cell_measurement_theta_max 68.21 _exptl_crystal_description 'subhedral rod' _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 1.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.645 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_process_details 'Sadabs in APEX2 (BrukerAXS, 2006)' _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 5.6 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 32152 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 68.21 _reflns_number_total 8163 _reflns_number_gt 7758 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 2008)' _computing_publication_material ; SHELX-97 (Sheldrick, 2008) and local procedures ; _publ_section_exptl_refinement ; H atoms were found in difference Fourier maps and subsequently placed in idealized positions with constrained distances of 0.98 \%A (RCH~3~), 0.99 \%A (R~2~CH~2~), 0.95 \%A (C~Ar~H), and with U~iso~(H) values set to either 1.2U~eq~ or 1.5U~eq~ (RCH~3~) of the attached atom. ; _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^)+(0.0540P)^2^+1.0456P] 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 8163 _refine_ls_number_parameters 539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.22576(3) 0.01747(3) 0.67228(3) 0.01786(10) Uani 1 1 d . . . Si2 Si 0.37113(3) 0.88774(3) 0.21176(3) 0.01601(10) Uani 1 1 d . . . N1 N -0.27206(10) 0.60833(9) 0.70358(8) 0.0174(2) Uani 1 1 d . . . N2 N 1.06098(10) 0.52179(9) 0.09518(8) 0.0183(2) Uani 1 1 d . . . O1 O -0.29606(9) 0.43742(7) 0.78832(7) 0.0201(2) Uani 1 1 d . . . O2 O 1.03468(9) 0.35374(7) 0.19827(7) 0.0209(2) Uani 1 1 d . . . C1 C 0.36145(12) 0.34560(10) 0.51924(9) 0.0144(3) Uani 1 1 d . . . C2 C 0.26740(12) 0.40474(10) 0.53661(9) 0.0143(3) Uani 1 1 d . . . C3 C 0.15690(12) 0.35923(10) 0.61094(9) 0.0156(3) Uani 1 1 d . . . H3 H 0.1445 0.2877 0.6508 0.019 Uiso 1 1 calc R . . C4 C 0.06843(12) 0.41937(10) 0.62468(9) 0.0154(3) Uani 1 1 d . . . S5 S -0.07214(3) 0.38032(2) 0.71227(2) 0.01610(9) Uani 1 1 d . . . C6 C -0.10961(12) 0.50664(10) 0.66965(9) 0.0155(3) Uani 1 1 d . . . C7 C -0.02160(12) 0.57424(11) 0.59226(10) 0.0166(3) Uani 1 1 d . . . H7 H -0.0284 0.6452 0.5597 0.020 Uiso 1 1 calc R . . C8 C 0.08292(12) 0.52713(10) 0.56483(9) 0.0149(3) Uani 1 1 d . . . C9 C 0.18890(12) 0.57258(10) 0.49208(9) 0.0146(3) Uani 1 1 d . . . H9 H 0.1985 0.6441 0.4519 0.017 Uiso 1 1 calc R . . C10 C 0.28358(12) 0.51351(10) 0.47679(9) 0.0138(3) Uani 1 1 d . . . C11 C 0.39348(12) 0.55978(10) 0.40255(9) 0.0139(3) Uani 1 1 d . . . C12 C 0.48980(12) 0.50109(10) 0.38913(9) 0.0137(3) Uani 1 1 d . . . C13 C 0.60020(12) 0.54776(10) 0.31628(9) 0.0150(3) Uani 1 1 d . . . H13 H 0.6122 0.6196 0.2787 0.018 Uiso 1 1 calc R . . C14 C 0.69039(12) 0.48965(10) 0.29954(9) 0.0153(3) Uani 1 1 d . . . C15 C 0.80589(12) 0.52334(11) 0.22653(10) 0.0173(3) Uani 1 1 d . . . H15 H 0.8322 0.5926 0.1812 0.021 Uiso 1 1 calc R . . C16 C 0.87328(12) 0.44532(10) 0.22947(9) 0.0158(3) Uani 1 1 d . . . S17 S 0.80085(3) 0.32577(2) 0.32225(2) 0.01701(9) Uani 1 1 d . . . C18 C 0.67408(12) 0.38175(10) 0.35829(10) 0.0159(3) Uani 1 1 d . . . C19 C 0.57007(12) 0.33391(10) 0.43199(10) 0.0155(3) Uani 1 1 d . . . H19 H 0.5623 0.2624 0.4719 0.019 Uiso 1 1 calc R . . C20 C 0.47399(12) 0.39232(10) 0.44815(9) 0.0142(3) Uani 1 1 d . . . C21 C 0.33675(11) 0.23736(10) 0.57042(9) 0.0151(3) Uani 1 1 d . . . C22 C 0.30390(12) 0.14720(10) 0.61160(10) 0.0174(3) Uani 1 1 d . . . C23 C 0.33541(14) -0.07280(11) 0.65496(12) 0.0258(3) Uani 1 1 d . . . H23A H 0.4157 -0.0572 0.6644 0.031 Uiso 1 1 calc R . . H23B H 0.3030 -0.1429 0.7057 0.031 Uiso 1 1 calc R . . C24 C 0.35566(15) -0.06783(12) 0.55381(13) 0.0302(3) Uani 1 1 d . . . H24A H 0.2794 -0.0937 0.5479 0.045 Uiso 1 1 calc R . . H24B H 0.4218 -0.1094 0.5455 0.045 Uiso 1 1 calc R . . H24C H 0.3787 0.0028 0.5031 0.045 Uiso 1 1 calc R . . C25 C 0.09626(13) 0.02480(11) 0.61240(11) 0.0232(3) Uani 1 1 d . . . H25A H 0.0429 0.0759 0.6197 0.028 Uiso 1 1 calc R . . H25B H 0.1314 0.0491 0.5414 0.028 Uiso 1 1 calc R . . C26 C 0.01623(14) -0.07564(12) 0.65339(13) 0.0294(3) Uani 1 1 d . . . H26A H 0.0686 -0.1281 0.6501 0.044 Uiso 1 1 calc R . . H26B H -0.0443 -0.0666 0.6145 0.044 Uiso 1 1 calc R . . H26C H -0.0268 -0.0965 0.7218 0.044 Uiso 1 1 calc R . . C27 C 0.16387(14) -0.02056(12) 0.80534(11) 0.0266(3) Uani 1 1 d . . . H27A H 0.1145 -0.0873 0.8365 0.032 Uiso 1 1 calc R . . H27B H 0.2342 -0.0297 0.8360 0.032 Uiso 1 1 calc R . . C28 C 0.08423(17) 0.05373(15) 0.82797(13) 0.0382(4) Uani 1 1 d . . . H28A H 0.1343 0.1181 0.8037 0.057 Uiso 1 1 calc R . . H28B H 0.0512 0.0250 0.8990 0.057 Uiso 1 1 calc R . . H28C H 0.0160 0.0659 0.7958 0.057 Uiso 1 1 calc R . . C29 C 0.40307(11) 0.66633(10) 0.33888(9) 0.0145(3) Uani 1 1 d . . . C30 C 0.40153(12) 0.75550(10) 0.28516(10) 0.0168(3) Uani 1 1 d . . . C31 C 0.36089(13) 0.90939(11) 0.08726(10) 0.0209(3) Uani 1 1 d . . . H31A H 0.3446 0.9808 0.0500 0.025 Uiso 1 1 calc R . . H31B H 0.4422 0.9007 0.0527 0.025 Uiso 1 1 calc R . . C32 C 0.26287(15) 0.84065(12) 0.08446(11) 0.0287(3) Uani 1 1 d . . . H32A H 0.2797 0.7696 0.1184 0.043 Uiso 1 1 calc R . . H32B H 0.2648 0.8589 0.0161 0.043 Uiso 1 1 calc R . . H32C H 0.1813 0.8494 0.1171 0.043 Uiso 1 1 calc R . . C33 C 0.49979(14) 0.97551(11) 0.19986(11) 0.0224(3) Uani 1 1 d . . . H33A H 0.5182 0.9516 0.2648 0.027 Uiso 1 1 calc R . . H33B H 0.5745 0.9716 0.1546 0.027 Uiso 1 1 calc R . . C34 C 0.47244(15) 1.08664(11) 0.16225(12) 0.0272(3) Uani 1 1 d . . . H34A H 0.4514 1.1105 0.0989 0.041 Uiso 1 1 calc R . . H34B H 0.5454 1.1282 0.1542 0.041 Uiso 1 1 calc R . . H34C H 0.4031 1.0923 0.2095 0.041 Uiso 1 1 calc R . . C35 C 0.22192(13) 0.90323(12) 0.28404(11) 0.0240(3) Uani 1 1 d . . . H35A H 0.1962 0.9711 0.2457 0.029 Uiso 1 1 calc R . . H35B H 0.1576 0.8516 0.2946 0.029 Uiso 1 1 calc R . . C36 C 0.23141(15) 0.89221(13) 0.38371(12) 0.0291(3) Uani 1 1 d . . . H36A H 0.2595 0.8260 0.4211 0.044 Uiso 1 1 calc R . . H36B H 0.1503 0.8972 0.4201 0.044 Uiso 1 1 calc R . . H36C H 0.2905 0.9464 0.3736 0.044 Uiso 1 1 calc R . . C37 C -0.23211(12) 0.51594(10) 0.72450(9) 0.0160(3) Uani 1 1 d . . . C38 C -0.39615(12) 0.61358(11) 0.75639(10) 0.0198(3) Uani 1 1 d . . . H38A H -0.4018 0.5859 0.8274 0.024 Uiso 1 1 calc R . . H38B H -0.4596 0.5755 0.7470 0.024 Uiso 1 1 calc R . . C39 C -0.41146(13) 0.72669(11) 0.71021(11) 0.0230(3) Uani 1 1 d . . . H39A H -0.4656 0.7447 0.7580 0.028 Uiso 1 1 calc R . . H39B H -0.4464 0.7475 0.6524 0.028 Uiso 1 1 calc R . . C40 C -0.28010(13) 0.77612(11) 0.68035(11) 0.0223(3) Uani 1 1 d . . . H40A H -0.2556 0.7756 0.7371 0.027 Uiso 1 1 calc R . . H40B H -0.2717 0.8471 0.6280 0.027 Uiso 1 1 calc R . . C41 C -0.20267(13) 0.70972(10) 0.64320(10) 0.0188(3) Uani 1 1 d . . . H41A H -0.1967 0.7334 0.5726 0.023 Uiso 1 1 calc R . . H41B H -0.1186 0.7093 0.6537 0.023 Uiso 1 1 calc R . . C42 C 0.99559(12) 0.43802(10) 0.17267(10) 0.0167(3) Uani 1 1 d . . . C43 C 1.02795(13) 0.62692(11) 0.05237(10) 0.0208(3) Uani 1 1 d . . . H43A H 1.0279 0.6571 0.0970 0.025 Uiso 1 1 calc R . . H43B H 0.9457 0.6298 0.0383 0.025 Uiso 1 1 calc R . . C44 C 1.12869(14) 0.68183(12) -0.04208(11) 0.0272(3) Uani 1 1 d . . . H44A H 1.1050 0.6791 -0.0978 0.033 Uiso 1 1 calc R . . H44B H 1.1461 0.7538 -0.0581 0.033 Uiso 1 1 calc R . . C45 C 1.23944(14) 0.62295(12) -0.01843(12) 0.0285(3) Uani 1 1 d . . . H45A H 1.2814 0.6449 0.0191 0.034 Uiso 1 1 calc R . . H45B H 1.2994 0.6321 -0.0790 0.034 Uiso 1 1 calc R . . C46 C 1.18316(13) 0.51279(12) 0.04328(11) 0.0226(3) Uani 1 1 d . . . H46A H 1.1765 0.4807 0.0013 0.027 Uiso 1 1 calc R . . H46B H 1.2328 0.4725 0.0899 0.027 Uiso 1 1 calc R . . C1T C 0.64401(13) 0.69830(12) 0.01479(10) 0.0229(3) Uani 1 1 d . . . C2T C 0.60993(14) 0.73254(12) 0.08440(11) 0.0254(3) Uani 1 1 d . . . H2T H 0.5322 0.7079 0.1304 0.030 Uiso 1 1 calc R . . C3T C 0.68701(17) 0.80180(13) 0.08803(12) 0.0328(4) Uani 1 1 d . . . H3T H 0.6629 0.8232 0.1372 0.039 Uiso 1 1 calc R . . C4T C 0.79961(17) 0.84015(13) 0.01994(14) 0.0368(4) Uani 1 1 d . . . H4T H 0.8525 0.8883 0.0219 0.044 Uiso 1 1 calc R . . C5T C 0.83414(15) 0.80765(13) -0.05074(12) 0.0321(4) Uani 1 1 d . . . H5T H 0.9108 0.8341 -0.0979 0.038 Uiso 1 1 calc R . . C6T C 0.75757(14) 0.73677(12) -0.05319(11) 0.0254(3) Uani 1 1 d . . . H6T H 0.7825 0.7142 -0.1015 0.030 Uiso 1 1 calc R . . C7T C 0.55912(15) 0.62237(15) 0.01244(13) 0.0365(4) Uani 1 1 d . . . H7T1 H 0.4817 0.6083 0.0621 0.055 Uiso 1 1 calc R . . H7T2 H 0.5982 0.5593 0.0263 0.055 Uiso 1 1 calc R . . H7T3 H 0.5421 0.6500 -0.0526 0.055 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 0.01683(19) 0.01403(19) 0.0186(2) -0.00361(15) -0.00494(14) -0.00247(14) Si2 0.01622(18) 0.01444(19) 0.01403(18) -0.00380(15) -0.00346(14) 0.00066(14) N1 0.0133(5) 0.0206(6) 0.0162(6) -0.0080(5) -0.0009(4) -0.0001(4) N2 0.0135(5) 0.0222(6) 0.0154(6) -0.0067(5) -0.0007(4) 0.0008(4) O1 0.0164(5) 0.0217(5) 0.0174(5) -0.0073(4) 0.0014(4) -0.0024(4) O2 0.0179(5) 0.0216(5) 0.0202(5) -0.0083(4) -0.0024(4) 0.0042(4) C1 0.0144(6) 0.0160(7) 0.0115(6) -0.0048(5) -0.0040(5) -0.0015(5) C2 0.0136(6) 0.0169(6) 0.0119(6) -0.0058(5) -0.0043(5) -0.0014(5) C3 0.0152(6) 0.0156(6) 0.0132(6) -0.0042(5) -0.0033(5) -0.0021(5) C4 0.0134(6) 0.0193(7) 0.0115(6) -0.0054(5) -0.0025(5) -0.0026(5) S5 0.01256(16) 0.01742(17) 0.01389(17) -0.00494(13) 0.00022(12) -0.00157(12) C6 0.0145(6) 0.0183(7) 0.0136(6) -0.0070(5) -0.0038(5) -0.0004(5) C7 0.0128(6) 0.0227(7) 0.0144(6) -0.0089(6) -0.0029(5) -0.0001(5) C8 0.0135(6) 0.0189(7) 0.0131(6) -0.0077(5) -0.0040(5) 0.0000(5) C9 0.0144(6) 0.0156(6) 0.0123(6) -0.0053(5) -0.0029(5) -0.0007(5) C10 0.0128(6) 0.0170(6) 0.0114(6) -0.0061(5) -0.0032(5) -0.0011(5) C11 0.0138(6) 0.0159(6) 0.0113(6) -0.0055(5) -0.0032(5) -0.0015(5) C12 0.0128(6) 0.0165(6) 0.0117(6) -0.0061(5) -0.0036(5) -0.0005(5) C13 0.0145(6) 0.0152(6) 0.0131(6) -0.0049(5) -0.0027(5) -0.0014(5) C14 0.0128(6) 0.0188(7) 0.0136(6) -0.0071(5) -0.0030(5) -0.0008(5) C15 0.0122(6) 0.0217(7) 0.0178(7) -0.0094(6) -0.0024(5) -0.0004(5) C16 0.0138(6) 0.0179(7) 0.0139(6) -0.0062(5) -0.0025(5) -0.0012(5) S17 0.01363(16) 0.01667(17) 0.01770(17) -0.00679(14) -0.00054(12) 0.00021(12) C18 0.0146(6) 0.0194(7) 0.0157(6) -0.0092(5) -0.0050(5) 0.0012(5) C19 0.0149(6) 0.0152(6) 0.0154(6) -0.0059(5) -0.0044(5) -0.0006(5) C20 0.0134(6) 0.0176(6) 0.0116(6) -0.0062(5) -0.0041(5) -0.0009(5) C21 0.0109(6) 0.0193(7) 0.0141(6) -0.0074(5) -0.0019(5) 0.0003(5) C22 0.0145(6) 0.0191(7) 0.0164(6) -0.0067(6) -0.0027(5) 0.0002(5) C23 0.0265(8) 0.0180(7) 0.0340(8) -0.0106(6) -0.0127(6) 0.0014(6) C24 0.0267(8) 0.0280(8) 0.0382(9) -0.0177(7) -0.0072(7) 0.0017(6) C25 0.0203(7) 0.0214(7) 0.0253(8) -0.0074(6) -0.0079(6) -0.0008(6) C26 0.0218(7) 0.0287(8) 0.0372(9) -0.0136(7) -0.0093(6) -0.0041(6) C27 0.0238(7) 0.0252(8) 0.0201(7) -0.0015(6) -0.0046(6) -0.0088(6) C28 0.0403(10) 0.0469(11) 0.0244(8) -0.0166(8) -0.0016(7) -0.0008(8) C29 0.0100(6) 0.0191(7) 0.0130(6) -0.0073(6) -0.0001(5) -0.0007(5) C30 0.0132(6) 0.0198(7) 0.0146(6) -0.0068(6) -0.0005(5) -0.0012(5) C31 0.0220(7) 0.0193(7) 0.0152(7) -0.0032(6) -0.0034(5) -0.0015(5) C32 0.0302(8) 0.0329(8) 0.0191(7) -0.0089(7) -0.0050(6) -0.0072(7) C33 0.0242(7) 0.0177(7) 0.0232(7) -0.0062(6) -0.0090(6) 0.0005(5) C34 0.0371(9) 0.0183(7) 0.0250(8) -0.0080(6) -0.0094(7) 0.0001(6) C35 0.0215(7) 0.0285(8) 0.0215(7) -0.0109(6) -0.0062(6) 0.0075(6) C36 0.0275(8) 0.0375(9) 0.0240(8) -0.0159(7) -0.0061(6) 0.0094(7) C37 0.0142(6) 0.0213(7) 0.0126(6) -0.0081(5) -0.0030(5) -0.0010(5) C38 0.0135(6) 0.0271(8) 0.0203(7) -0.0133(6) -0.0015(5) 0.0022(5) C39 0.0189(7) 0.0282(8) 0.0260(8) -0.0157(6) -0.0062(6) 0.0054(6) C40 0.0223(7) 0.0229(7) 0.0243(7) -0.0129(6) -0.0061(6) 0.0027(6) C41 0.0181(7) 0.0189(7) 0.0178(7) -0.0074(6) -0.0038(5) 0.0003(5) C42 0.0148(6) 0.0218(7) 0.0142(6) -0.0084(6) -0.0045(5) 0.0003(5) C43 0.0204(7) 0.0207(7) 0.0172(7) -0.0062(6) -0.0024(6) 0.0002(5) C44 0.0258(8) 0.0278(8) 0.0200(7) -0.0062(6) -0.0009(6) -0.0032(6) C45 0.0191(7) 0.0326(9) 0.0243(8) -0.0079(7) 0.0014(6) -0.0039(6) C46 0.0141(7) 0.0311(8) 0.0188(7) -0.0101(6) 0.0001(5) 0.0018(6) C1T 0.0198(7) 0.0278(8) 0.0167(7) -0.0065(6) -0.0046(5) 0.0069(6) C2T 0.0259(8) 0.0277(8) 0.0159(7) -0.0053(6) -0.0035(6) 0.0088(6) C3T 0.0420(10) 0.0294(8) 0.0269(8) -0.0133(7) -0.0081(7) 0.0096(7) C4T 0.0403(10) 0.0264(8) 0.0397(10) -0.0105(8) -0.0127(8) 0.0000(7) C5T 0.0235(8) 0.0301(8) 0.0257(8) -0.0006(7) -0.0013(6) 0.0007(6) C6T 0.0225(7) 0.0319(8) 0.0159(7) -0.0071(6) -0.0029(6) 0.0073(6) C7T 0.0235(8) 0.0527(11) 0.0352(9) -0.0256(9) 0.0012(7) -0.0024(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C22 1.8415(14) . ? Si1 C27 1.8682(16) . ? Si1 C23 1.8720(16) . ? Si1 C25 1.8753(15) . ? Si2 C30 1.8447(14) . ? Si2 C31 1.8710(14) . ? Si2 C35 1.8740(15) . ? Si2 C33 1.8750(15) . ? N1 C37 1.3509(18) . ? N1 C38 1.4711(17) . ? N1 C41 1.4757(18) . ? N2 C42 1.3504(18) . ? N2 C46 1.4656(17) . ? N2 C43 1.4715(18) . ? O1 C37 1.2336(17) . ? O2 C42 1.2339(17) . ? C1 C20 1.4184(18) . ? C1 C2 1.4188(18) . ? C1 C21 1.4302(19) . ? C2 C3 1.4200(18) . ? C2 C10 1.4421(19) . ? C3 C4 1.3693(19) . ? C3 H3 0.9500 . ? C4 C8 1.4300(19) . ? C4 S5 1.7451(13) . ? S5 C6 1.7609(14) . ? C6 C7 1.3591(19) . ? C6 C37 1.4888(18) . ? C7 C8 1.4372(19) . ? C7 H7 0.9500 . ? C8 C9 1.3748(19) . ? C9 C10 1.4131(19) . ? C9 H9 0.9500 . ? C10 C11 1.4162(18) . ? C11 C12 1.4144(18) . ? C11 C29 1.4273(19) . ? C12 C13 1.4121(18) . ? C12 C20 1.4406(19) . ? C13 C14 1.3752(19) . ? C13 H13 0.9500 . ? C14 C18 1.4295(19) . ? C14 C15 1.4410(19) . ? C15 C16 1.360(2) . ? C15 H15 0.9500 . ? C16 C42 1.4902(19) . ? C16 S17 1.7618(13) . ? S17 C18 1.7478(14) . ? C18 C19 1.3711(19) . ? C19 C20 1.4214(19) . ? C19 H19 0.9500 . ? C21 C22 1.211(2) . ? C23 C24 1.528(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.532(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.523(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.208(2) . ? C31 C32 1.530(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.531(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.533(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C38 C39 1.522(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.526(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.5278(19) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C43 C44 1.526(2) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.522(2) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.526(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C1T C2T 1.386(2) . ? C1T C6T 1.395(2) . ? C1T C7T 1.503(2) . ? C2T C3T 1.380(2) . ? C2T H2T 0.9500 . ? C3T C4T 1.388(3) . ? C3T H3T 0.9500 . ? C4T C5T 1.383(3) . ? C4T H4T 0.9500 . ? C5T C6T 1.386(2) . ? C5T H5T 0.9500 . ? C6T H6T 0.9500 . ? C7T H7T1 0.9800 . ? C7T H7T2 0.9800 . ? C7T H7T3 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 C22 Si1 C27 108.52(7) . . ? C22 Si1 C23 110.38(7) . . ? C27 Si1 C23 110.92(7) . . ? C22 Si1 C25 105.77(6) . . ? C27 Si1 C25 110.36(7) . . ? C23 Si1 C25 110.75(7) . . ? C30 Si2 C31 110.39(6) . . ? C30 Si2 C35 104.86(6) . . ? C31 Si2 C35 112.06(7) . . ? C30 Si2 C33 108.72(6) . . ? C31 Si2 C33 109.79(7) . . ? C35 Si2 C33 110.89(7) . . ? C37 N1 C38 118.49(11) . . ? C37 N1 C41 129.08(11) . . ? C38 N1 C41 111.87(11) . . ? C42 N2 C46 119.12(12) . . ? C42 N2 C43 128.99(12) . . ? C46 N2 C43 111.89(11) . . ? C20 C1 C2 120.98(12) . . ? C20 C1 C21 120.61(12) . . ? C2 C1 C21 118.27(11) . . ? C1 C2 C3 121.53(12) . . ? C1 C2 C10 119.34(12) . . ? C3 C2 C10 119.13(12) . . ? C4 C3 C2 119.45(12) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C8 121.82(12) . . ? C3 C4 S5 127.21(10) . . ? C8 C4 S5 110.97(10) . . ? C4 S5 C6 91.13(6) . . ? C7 C6 C37 133.90(13) . . ? C7 C6 S5 112.95(10) . . ? C37 C6 S5 113.13(10) . . ? C6 C7 C8 112.91(12) . . ? C6 C7 H7 123.5 . . ? C8 C7 H7 123.5 . . ? C9 C8 C4 119.62(12) . . ? C9 C8 C7 128.36(13) . . ? C4 C8 C7 112.02(12) . . ? C8 C9 C10 120.37(12) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 C11 120.75(12) . . ? C9 C10 C2 119.61(12) . . ? C11 C10 C2 119.64(12) . . ? C12 C11 C10 120.77(12) . . ? C12 C11 C29 120.58(12) . . ? C10 C11 C29 118.60(12) . . ? C13 C12 C11 120.61(12) . . ? C13 C12 C20 119.51(12) . . ? C11 C12 C20 119.85(12) . . ? C14 C13 C12 120.31(12) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C18 119.87(12) . . ? C13 C14 C15 128.02(13) . . ? C18 C14 C15 112.10(12) . . ? C16 C15 C14 112.76(12) . . ? C16 C15 H15 123.6 . . ? C14 C15 H15 123.6 . . ? C15 C16 C42 134.48(13) . . ? C15 C16 S17 113.04(10) . . ? C42 C16 S17 112.47(10) . . ? C18 S17 C16 91.14(6) . . ? C19 C18 C14 121.55(12) . . ? C19 C18 S17 127.51(11) . . ? C14 C18 S17 110.95(10) . . ? C18 C19 C20 119.38(12) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C1 C20 C19 121.42(12) . . ? C1 C20 C12 119.24(12) . . ? C19 C20 C12 119.31(12) . . ? C22 C21 C1 173.19(14) . . ? C21 C22 Si1 169.55(12) . . ? C24 C23 Si1 113.03(11) . . ? C24 C23 H23A 109.0 . . ? Si1 C23 H23A 109.0 . . ? C24 C23 H23B 109.0 . . ? Si1 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 Si1 114.77(10) . . ? C26 C25 H25A 108.6 . . ? Si1 C25 H25A 108.6 . . ? C26 C25 H25B 108.6 . . ? Si1 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 Si1 115.46(11) . . ? C28 C27 H27A 108.4 . . ? Si1 C27 H27A 108.4 . . ? C28 C27 H27B 108.4 . . ? Si1 C27 H27B 108.4 . . ? H27A C27 H27B 107.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C11 174.85(14) . . ? C29 C30 Si2 170.44(12) . . ? C32 C31 Si2 116.24(10) . . ? C32 C31 H31A 108.2 . . ? Si2 C31 H31A 108.2 . . ? C32 C31 H31B 108.2 . . ? Si2 C31 H31B 108.2 . . ? H31A C31 H31B 107.4 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 Si2 114.26(10) . . ? C34 C33 H33A 108.7 . . ? Si2 C33 H33A 108.7 . . ? C34 C33 H33B 108.7 . . ? Si2 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? 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 . . ? C36 C35 Si2 112.54(10) . . ? C36 C35 H35A 109.1 . . ? Si2 C35 H35A 109.1 . . ? C36 C35 H35B 109.1 . . ? Si2 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O1 C37 N1 121.26(12) . . ? O1 C37 C6 118.32(12) . . ? N1 C37 C6 120.41(12) . . ? N1 C38 C39 103.66(11) . . ? N1 C38 H38A 111.0 . . ? C39 C38 H38A 111.0 . . ? N1 C38 H38B 111.0 . . ? C39 C38 H38B 111.0 . . ? H38A C38 H38B 109.0 . . ? C38 C39 C40 103.34(11) . . ? C38 C39 H39A 111.1 . . ? C40 C39 H39A 111.1 . . ? C38 C39 H39B 111.1 . . ? C40 C39 H39B 111.1 . . ? H39A C39 H39B 109.1 . . ? C39 C40 C41 103.52(11) . . ? C39 C40 H40A 111.1 . . ? C41 C40 H40A 111.1 . . ? C39 C40 H40B 111.1 . . ? C41 C40 H40B 111.1 . . ? H40A C40 H40B 109.0 . . ? N1 C41 C40 102.93(11) . . ? N1 C41 H41A 111.2 . . ? C40 C41 H41A 111.2 . . ? N1 C41 H41B 111.2 . . ? C40 C41 H41B 111.2 . . ? H41A C41 H41B 109.1 . . ? O2 C42 N2 121.35(12) . . ? O2 C42 C16 118.21(12) . . ? N2 C42 C16 120.44(12) . . ? N2 C43 C44 103.73(11) . . ? N2 C43 H43A 111.0 . . ? C44 C43 H43A 111.0 . . ? N2 C43 H43B 111.0 . . ? C44 C43 H43B 111.0 . . ? H43A C43 H43B 109.0 . . ? C45 C44 C43 103.37(12) . . ? C45 C44 H44A 111.1 . . ? C43 C44 H44A 111.1 . . ? C45 C44 H44B 111.1 . . ? C43 C44 H44B 111.1 . . ? H44A C44 H44B 109.1 . . ? C44 C45 C46 103.56(12) . . ? C44 C45 H45A 111.0 . . ? C46 C45 H45A 111.0 . . ? C44 C45 H45B 111.0 . . ? C46 C45 H45B 111.0 . . ? H45A C45 H45B 109.0 . . ? N2 C46 C45 103.20(12) . . ? N2 C46 H46A 111.1 . . ? C45 C46 H46A 111.1 . . ? N2 C46 H46B 111.1 . . ? C45 C46 H46B 111.1 . . ? H46A C46 H46B 109.1 . . ? C2T C1T C6T 118.56(15) . . ? C2T C1T C7T 120.31(14) . . ? C6T C1T C7T 121.13(14) . . ? C3T C2T C1T 121.11(15) . . ? C3T C2T H2T 119.4 . . ? C1T C2T H2T 119.4 . . ? C2T C3T C4T 120.07(16) . . ? C2T C3T H3T 120.0 . . ? C4T C3T H3T 120.0 . . ? C5T C4T C3T 119.44(16) . . ? C5T C4T H4T 120.3 . . ? C3T C4T H4T 120.3 . . ? C4T C5T C6T 120.40(15) . . ? C4T C5T H5T 119.8 . . ? C6T C5T H5T 119.8 . . ? C5T C6T C1T 120.40(15) . . ? C5T C6T H6T 119.8 . . ? C1T C6T H6T 119.8 . . ? C1T C7T H7T1 109.5 . . ? C1T C7T H7T2 109.5 . . ? H7T1 C7T H7T2 109.5 . . ? C1T C7T H7T3 109.5 . . ? H7T1 C7T H7T3 109.5 . . ? H7T2 C7T H7T3 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 C20 C1 C2 C3 -176.79(11) . . . . ? C21 C1 C2 C3 7.42(18) . . . . ? C20 C1 C2 C10 3.90(18) . . . . ? C21 C1 C2 C10 -171.89(11) . . . . ? C1 C2 C3 C4 -179.67(11) . . . . ? C10 C2 C3 C4 -0.36(18) . . . . ? C2 C3 C4 C8 1.26(19) . . . . ? C2 C3 C4 S5 -178.85(10) . . . . ? C3 C4 S5 C6 179.62(12) . . . . ? C8 C4 S5 C6 -0.48(10) . . . . ? C4 S5 C6 C7 1.12(10) . . . . ? C4 S5 C6 C37 179.66(10) . . . . ? C37 C6 C7 C8 -179.60(13) . . . . ? S5 C6 C7 C8 -1.46(15) . . . . ? C3 C4 C8 C9 -0.86(19) . . . . ? S5 C4 C8 C9 179.24(10) . . . . ? C3 C4 C8 C7 179.68(12) . . . . ? S5 C4 C8 C7 -0.23(13) . . . . ? C6 C7 C8 C9 -178.32(13) . . . . ? C6 C7 C8 C4 1.09(16) . . . . ? C4 C8 C9 C10 -0.48(19) . . . . ? C7 C8 C9 C10 178.88(12) . . . . ? C8 C9 C10 C11 -179.48(11) . . . . ? C8 C9 C10 C2 1.36(18) . . . . ? C1 C2 C10 C9 178.39(11) . . . . ? C3 C2 C10 C9 -0.94(18) . . . . ? C1 C2 C10 C11 -0.78(18) . . . . ? C3 C2 C10 C11 179.89(11) . . . . ? C9 C10 C11 C12 178.10(11) . . . . ? C2 C10 C11 C12 -2.74(18) . . . . ? C9 C10 C11 C29 -4.42(18) . . . . ? C2 C10 C11 C29 174.74(11) . . . . ? C10 C11 C12 C13 -178.76(11) . . . . ? C29 C11 C12 C13 3.81(18) . . . . ? C10 C11 C12 C20 3.15(18) . . . . ? C29 C11 C12 C20 -174.27(11) . . . . ? C11 C12 C13 C14 -175.98(11) . . . . ? C20 C12 C13 C14 2.11(19) . . . . ? C12 C13 C14 C18 -2.05(19) . . . . ? C12 C13 C14 C15 177.45(12) . . . . ? C13 C14 C15 C16 -179.31(13) . . . . ? C18 C14 C15 C16 0.22(16) . . . . ? C14 C15 C16 C42 -179.64(13) . . . . ? C14 C15 C16 S17 -0.56(15) . . . . ? C15 C16 S17 C18 0.58(11) . . . . ? C42 C16 S17 C18 179.87(10) . . . . ? C13 C14 C18 C19 -0.24(19) . . . . ? C15 C14 C18 C19 -179.82(12) . . . . ? C13 C14 C18 S17 179.79(10) . . . . ? C15 C14 C18 S17 0.22(14) . . . . ? C16 S17 C18 C19 179.60(12) . . . . ? C16 S17 C18 C14 -0.44(10) . . . . ? C14 C18 C19 C20 2.41(19) . . . . ? S17 C18 C19 C20 -177.63(9) . . . . ? C2 C1 C20 C19 178.33(11) . . . . ? C21 C1 C20 C19 -5.98(18) . . . . ? C2 C1 C20 C12 -3.49(18) . . . . ? C21 C1 C20 C12 172.21(11) . . . . ? C18 C19 C20 C1 175.89(11) . . . . ? C18 C19 C20 C12 -2.29(18) . . . . ? C13 C12 C20 C1 -178.16(11) . . . . ? C11 C12 C20 C1 -0.05(18) . . . . ? C13 C12 C20 C19 0.07(18) . . . . ? C11 C12 C20 C19 178.17(11) . . . . ? C27 Si1 C22 C21 -85.7(7) . . . . ? C23 Si1 C22 C21 152.5(7) . . . . ? C25 Si1 C22 C21 32.7(7) . . . . ? C22 Si1 C23 C24 -78.75(12) . . . . ? C27 Si1 C23 C24 160.93(11) . . . . ? C25 Si1 C23 C24 38.04(13) . . . . ? C22 Si1 C25 C26 -178.90(11) . . . . ? C27 Si1 C25 C26 -61.72(13) . . . . ? C23 Si1 C25 C26 61.50(13) . . . . ? C22 Si1 C27 C28 52.34(13) . . . . ? C23 Si1 C27 C28 173.76(11) . . . . ? C25 Si1 C27 C28 -63.13(13) . . . . ? C30 Si2 C31 C32 58.04(13) . . . . ? C35 Si2 C31 C32 -58.43(13) . . . . ? C33 Si2 C31 C32 177.88(11) . . . . ? C30 Si2 C33 C34 -166.18(10) . . . . ? C31 Si2 C33 C34 72.96(12) . . . . ? C35 Si2 C33 C34 -51.40(13) . . . . ? C30 Si2 C35 C36 63.80(12) . . . . ? C31 Si2 C35 C36 -176.43(11) . . . . ? C33 Si2 C35 C36 -53.37(13) . . . . ? C38 N1 C37 O1 -2.08(19) . . . . ? C41 N1 C37 O1 168.55(12) . . . . ? C38 N1 C37 C6 177.11(11) . . . . ? C41 N1 C37 C6 -12.3(2) . . . . ? C7 C6 C37 O1 174.44(14) . . . . ? S5 C6 C37 O1 -3.69(15) . . . . ? C7 C6 C37 N1 -4.8(2) . . . . ? S5 C6 C37 N1 177.09(10) . . . . ? C37 N1 C38 C39 -176.80(11) . . . . ? C41 N1 C38 C39 11.03(14) . . . . ? N1 C38 C39 C40 -30.44(13) . . . . ? C38 C39 C40 C41 38.76(14) . . . . ? C37 N1 C41 C40 -158.24(13) . . . . ? C38 N1 C41 C40 12.89(14) . . . . ? C39 C40 C41 N1 -31.51(14) . . . . ? C46 N2 C42 O2 -2.67(19) . . . . ? C43 N2 C42 O2 177.88(12) . . . . ? C46 N2 C42 C16 177.55(12) . . . . ? C43 N2 C42 C16 -1.9(2) . . . . ? C15 C16 C42 O2 175.64(14) . . . . ? S17 C16 C42 O2 -3.45(15) . . . . ? C15 C16 C42 N2 -4.6(2) . . . . ? S17 C16 C42 N2 176.34(10) . . . . ? C42 N2 C43 C44 -171.08(13) . . . . ? C46 N2 C43 C44 9.45(15) . . . . ? N2 C43 C44 C45 -29.14(15) . . . . ? C43 C44 C45 C46 38.06(15) . . . . ? C42 N2 C46 C45 -165.46(12) . . . . ? C43 N2 C46 C45 14.08(15) . . . . ? C44 C45 C46 N2 -31.93(15) . . . . ? C6T C1T C2T C3T -1.1(2) . . . . ? C7T C1T C2T C3T 179.61(15) . . . . ? C1T C2T C3T C4T 1.5(2) . . . . ? C2T C3T C4T C5T -0.6(3) . . . . ? C3T C4T C5T C6T -0.5(2) . . . . ? C4T C5T C6T C1T 0.8(2) . . . . ? C2T C1T C6T C5T 0.0(2) . . . . ? C7T C1T C6T C5T 179.24(15) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 68.21 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.425 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.061