data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'George Malliaras' 'John E Anthony' 'Yee-Fun Lim' 'Sean Parkin' 'Ying Shu' _publ_contact_author_name 'George Malliaras' _publ_contact_author_email GGM1@CORNELL.EDU _publ_section_title ; Soluble n-type pentacene derivatives as novel acceptors for organic solar cells ; # Attachment 'Monocyano_TCPS.cif' data_x08034 _database_code_depnum_ccdc_archive 'CCDC 722603' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H64 N Si2' _chemical_formula_sum 'C55 H64 N Si2' _chemical_formula_weight 795.25 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' Si Si 0.2541 0.3302 '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 n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 16.8241(6) _cell_length_b 17.0411(9) _cell_length_c 16.1283(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4624.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 8296 _cell_measurement_theta_min 3.77 _cell_measurement_theta_max 68.49 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 0.960 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8462 _exptl_absorpt_correction_T_max 0.9446 _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 18 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 65241 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 69.04 _reflns_number_total 4431 _reflns_number_gt 2611 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker-AXS, 2006)' _computing_data_reduction 'APEX2 (Bruker-AXS, 2006)' _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 ; SHELX97-2 (Sheldrick, 2008) 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^)+(0.1572P)^2^+18.3579P] 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 4431 _refine_ls_number_parameters 350 _refine_ls_number_restraints 423 _refine_ls_R_factor_all 0.1779 _refine_ls_R_factor_gt 0.1142 _refine_ls_wR_factor_ref 0.3801 _refine_ls_wR_factor_gt 0.2931 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.083 _refine_ls_shift/su_mean 0.005 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 0.72029(13) 0.2500 0.73905(15) 0.0674(8) Uani 1 2 d SU . . Si2 Si 0.15624(13) 0.2500 0.31823(17) 0.0697(8) Uani 1 2 d SU . . C1 C 0.4862(4) 0.2500 0.6073(5) 0.0580(16) Uani 1 2 d SU . . C2 C 0.4521(3) 0.3218(4) 0.5843(3) 0.0573(13) Uani 1 1 d U . . C3 C 0.4817(3) 0.3947(5) 0.6113(4) 0.0655(14) Uani 1 1 d U . . H3 H 0.5268 0.3952 0.6468 0.079 Uiso 1 1 calc R . . C4 C 0.4490(4) 0.4642(5) 0.5892(4) 0.0711(14) Uani 1 1 d U . . C5 C 0.4789(5) 0.5389(5) 0.6153(5) 0.0844(18) Uani 1 1 d U . . H5 H 0.5239 0.5402 0.6509 0.101 Uiso 1 1 calc R . . C6 C 0.4467(6) 0.6063(6) 0.5920(5) 0.0935(19) Uani 1 1 d U . . C7 C 0.3789(5) 0.6073(6) 0.5385(5) 0.0898(18) Uani 1 1 d U . . C8 C 0.3471(4) 0.5382(5) 0.5124(5) 0.0816(17) Uani 1 1 d U . . H8 H 0.3013 0.5394 0.4779 0.098 Uiso 1 1 calc R . . C9 C 0.3801(4) 0.4641(5) 0.5349(4) 0.0688(14) Uani 1 1 d U . . C10 C 0.3499(3) 0.3937(4) 0.5082(4) 0.0635(13) Uani 1 1 d U . . H10 H 0.3052 0.3936 0.4722 0.076 Uiso 1 1 calc R . . C11 C 0.3829(3) 0.3222(4) 0.5325(3) 0.0568(12) Uani 1 1 d U . . C12 C 0.3509(4) 0.2500 0.5049(5) 0.0581(17) Uani 1 2 d SU . . C13 C 0.5593(5) 0.2500 0.6528(6) 0.069(2) Uani 1 2 d SU . . C14 C 0.6223(5) 0.2500 0.6873(6) 0.068(2) Uani 1 2 d SU A . C15 C 0.8000(5) 0.2375(11) 0.6609(7) 0.070(3) Uani 0.50 1 d PDU A -1 H15 H 0.7849 0.1927 0.6241 0.084 Uiso 0.50 1 calc PR A -1 C16 C 0.8207(9) 0.3078(10) 0.6055(11) 0.099(4) Uani 0.50 1 d PDU A -1 H16A H 0.8223 0.3571 0.6380 0.119 Uiso 0.50 1 calc PR A -1 H16B H 0.7817 0.3136 0.5599 0.119 Uiso 0.50 1 calc PR A -1 C17 C 0.9026(8) 0.2869(10) 0.5722(10) 0.098(4) Uani 0.50 1 d PDU A -1 H17A H 0.9362 0.3344 0.5692 0.117 Uiso 0.50 1 calc PR A -1 H17B H 0.8979 0.2645 0.5157 0.117 Uiso 0.50 1 calc PR A -1 C18 C 0.9400(7) 0.2264(9) 0.6312(10) 0.094(5) Uani 0.50 1 d PDU A -1 H18A H 0.9483 0.1756 0.6027 0.113 Uiso 0.50 1 calc PR A -1 H18B H 0.9917 0.2454 0.6525 0.113 Uiso 0.50 1 calc PR A -1 C19 C 0.8807(6) 0.2185(9) 0.6999(8) 0.083(4) Uani 0.50 1 d PDU A -1 H19A H 0.8929 0.2556 0.7454 0.100 Uiso 0.50 1 calc PR A -1 H19B H 0.8810 0.1644 0.7224 0.100 Uiso 0.50 1 calc PR A -1 C20 C 0.7252(4) 0.3430(5) 0.7987(4) 0.0805(17) Uani 1 1 d DU A . H20 H 0.7801 0.3472 0.8222 0.097 Uiso 1 1 calc R . . C21 C 0.6675(5) 0.3507(5) 0.8703(5) 0.097(2) Uani 1 1 d DU . . H21A H 0.6902 0.3280 0.9215 0.117 Uiso 1 1 calc R A . H21B H 0.6168 0.3237 0.8576 0.117 Uiso 1 1 calc R . . C22 C 0.6544(6) 0.4389(6) 0.8800(6) 0.114(3) Uani 1 1 d DU A . H22A H 0.6049 0.4499 0.9112 0.136 Uiso 1 1 calc R . . H22B H 0.6997 0.4639 0.9089 0.136 Uiso 1 1 calc R . . C23 C 0.6483(7) 0.4666(6) 0.7936(7) 0.129(3) Uani 1 1 d DU . . H23A H 0.6607 0.5233 0.7897 0.155 Uiso 1 1 calc R A . H23B H 0.5943 0.4574 0.7712 0.155 Uiso 1 1 calc R . . C24 C 0.7099(5) 0.4177(5) 0.7474(6) 0.101(2) Uani 1 1 d DU A . H24A H 0.7598 0.4479 0.7408 0.121 Uiso 1 1 calc R . . H24B H 0.6899 0.4037 0.6916 0.121 Uiso 1 1 calc R . . C25 C 0.2854(4) 0.2500 0.4484(5) 0.058(2) Uani 1 2 d SU B . C26 C 0.2321(4) 0.2500 0.4009(5) 0.059(2) Uani 1 2 d SU B . C27 C 0.2124(6) 0.2362(9) 0.2176(7) 0.064(3) Uani 0.50 1 d PDU B -1 H27 H 0.1725 0.2352 0.1716 0.077 Uiso 0.50 1 calc PR B -1 C28 C 0.2645(11) 0.1639(9) 0.2088(13) 0.075(4) Uani 0.50 1 d PDU B -1 H28A H 0.2330 0.1172 0.1931 0.090 Uiso 0.50 1 calc PR B -1 H28B H 0.2941 0.1527 0.2606 0.090 Uiso 0.50 1 calc PR B -1 C29 C 0.3199(11) 0.1889(10) 0.1394(12) 0.098(5) Uani 0.50 1 d PDU B -1 H29A H 0.3693 0.1574 0.1405 0.118 Uiso 0.50 1 calc PR B -1 H29B H 0.2940 0.1819 0.0849 0.118 Uiso 0.50 1 calc PR B -1 C30 C 0.3383(10) 0.2745(8) 0.1543(13) 0.103(6) Uani 0.50 1 d PDU B -1 H30A H 0.3879 0.2804 0.1868 0.124 Uiso 0.50 1 calc PR B -1 H30B H 0.3444 0.3028 0.1011 0.124 Uiso 0.50 1 calc PR B -1 C31 C 0.2681(11) 0.3054(9) 0.2022(14) 0.078(4) Uani 0.50 1 d PDU B -1 H31A H 0.2405 0.3467 0.1700 0.094 Uiso 0.50 1 calc PR B -1 H31B H 0.2858 0.3282 0.2556 0.094 Uiso 0.50 1 calc PR B -1 C32 C 0.0943(4) 0.3384(5) 0.3300(5) 0.092(2) Uani 1 1 d DU B . H32 H 0.0526 0.3367 0.2859 0.111 Uiso 1 1 calc R . . C33 C 0.0519(6) 0.3433(6) 0.4131(6) 0.131(3) Uani 1 1 d DU . . H33A H 0.0889 0.3336 0.4597 0.158 Uiso 1 1 calc R B . H33B H 0.0073 0.3054 0.4162 0.158 Uiso 1 1 calc R . . C34 C 0.0221(8) 0.4273(7) 0.4129(9) 0.170(4) Uani 1 1 d DU B . H34A H -0.0292 0.4309 0.3832 0.204 Uiso 1 1 calc R . . H34B H 0.0142 0.4460 0.4705 0.204 Uiso 1 1 calc R . . C35 C 0.0841(8) 0.4764(7) 0.3699(9) 0.168(4) Uani 1 1 d DU . . H35A H 0.1163 0.5062 0.4106 0.201 Uiso 1 1 calc R B . H35B H 0.0591 0.5139 0.3308 0.201 Uiso 1 1 calc R . . C36 C 0.1356(6) 0.4167(6) 0.3233(7) 0.123(3) Uani 1 1 d DU B . H36A H 0.1412 0.4321 0.2644 0.148 Uiso 1 1 calc R . . H36B H 0.1892 0.4138 0.3483 0.148 Uiso 1 1 calc R . . C37 C 0.4937(11) 0.6760(12) 0.6289(10) 0.062(3) Uani 0.334(7) 1 d PU . 1 N1 N 0.5215(9) 0.7500 0.6525(9) 0.099(4) Uani 0.667(14) 2 d SPU . 1 C37' C 0.345(3) 0.669(3) 0.520(3) 0.082(6) Uani 0.166(7) 1 d PU . 2 N1' N 0.316(2) 0.7500 0.512(2) 0.120(7) Uani 0.333(14) 2 d SPU . 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 0.0366(11) 0.110(2) 0.0551(13) 0.000 -0.0089(9) 0.000 Si2 0.0305(10) 0.105(2) 0.0738(16) 0.000 -0.0069(10) 0.000 C1 0.031(3) 0.103(4) 0.040(4) 0.000 0.008(2) 0.000 C2 0.034(2) 0.097(3) 0.041(3) -0.001(3) 0.0072(18) -0.007(2) C3 0.045(3) 0.106(3) 0.046(3) -0.006(3) 0.005(2) -0.013(3) C4 0.057(3) 0.102(3) 0.054(3) -0.007(3) 0.018(2) -0.015(3) C5 0.078(4) 0.108(3) 0.067(4) -0.016(3) 0.026(3) -0.024(3) C6 0.096(4) 0.113(4) 0.072(4) -0.009(4) 0.038(3) -0.007(3) C7 0.086(4) 0.106(4) 0.078(4) -0.005(4) 0.044(3) -0.008(3) C8 0.068(4) 0.101(3) 0.076(4) 0.003(3) 0.028(3) 0.003(3) C9 0.051(3) 0.103(3) 0.052(3) 0.001(3) 0.020(2) -0.004(3) C10 0.039(3) 0.101(3) 0.050(3) 0.004(3) 0.007(2) -0.002(3) C11 0.031(2) 0.100(3) 0.040(3) 0.001(2) 0.0097(18) -0.003(2) C12 0.030(3) 0.097(4) 0.048(4) 0.000 0.006(2) 0.000 C13 0.037(3) 0.113(6) 0.056(4) 0.000 -0.002(3) 0.000 C14 0.043(3) 0.103(6) 0.057(5) 0.000 -0.005(3) 0.000 C15 0.047(3) 0.097(8) 0.066(5) 0.002(5) -0.008(3) 0.005(6) C16 0.081(7) 0.122(9) 0.095(8) 0.025(6) 0.021(5) 0.016(6) C17 0.076(6) 0.125(9) 0.091(7) 0.002(6) 0.017(6) 0.002(6) C18 0.058(5) 0.106(10) 0.117(8) -0.001(6) 0.010(5) -0.002(5) C19 0.048(4) 0.115(9) 0.086(6) 0.000(5) -0.008(4) 0.010(5) C20 0.051(3) 0.116(4) 0.075(4) -0.011(3) -0.016(3) 0.001(3) C21 0.087(5) 0.129(5) 0.076(4) -0.009(3) -0.007(3) 0.026(5) C22 0.090(5) 0.133(5) 0.118(4) -0.033(5) -0.031(4) 0.034(5) C23 0.133(7) 0.116(6) 0.138(6) -0.002(5) 0.008(6) 0.020(5) C24 0.076(4) 0.105(4) 0.121(5) 0.004(4) -0.002(4) -0.009(4) C25 0.032(3) 0.086(5) 0.055(4) 0.000 0.002(2) 0.000 C26 0.035(3) 0.079(5) 0.064(4) 0.000 -0.003(3) 0.000 C27 0.053(4) 0.072(8) 0.068(4) -0.002(5) -0.015(3) -0.001(4) C28 0.063(7) 0.080(7) 0.083(8) -0.001(7) 0.001(5) 0.007(6) C29 0.085(8) 0.112(8) 0.097(8) -0.023(7) 0.021(6) -0.014(7) C30 0.097(7) 0.100(9) 0.112(9) 0.004(7) 0.033(7) -0.007(6) C31 0.072(7) 0.081(7) 0.081(8) 0.007(7) 0.003(5) -0.009(6) C32 0.055(4) 0.125(4) 0.097(4) -0.005(4) -0.016(3) 0.023(3) C33 0.107(6) 0.164(6) 0.123(6) -0.026(5) 0.009(5) 0.047(5) C34 0.158(8) 0.171(7) 0.181(9) -0.036(6) 0.007(6) 0.064(6) C35 0.156(8) 0.142(5) 0.206(9) -0.032(6) -0.007(7) 0.056(6) C36 0.109(6) 0.111(4) 0.150(7) -0.025(5) -0.028(4) 0.016(4) C37 0.058(7) 0.087(5) 0.040(6) 0.019(6) 0.034(5) 0.025(5) N1 0.096(8) 0.123(6) 0.078(7) 0.000 0.015(6) 0.000 C37' 0.081(11) 0.097(5) 0.067(11) -0.016(9) 0.024(8) -0.025(8) N1' 0.122(12) 0.120(6) 0.117(13) 0.000 -0.007(10) 0.000 _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 C15 1.853(11) 7_565 ? Si1 C15 1.853(11) . ? Si1 C14 1.848(9) . ? Si1 C20 1.856(8) . ? Si1 C20 1.856(8) 7_565 ? Si2 C32 1.842(8) 7_565 ? Si2 C32 1.842(8) . ? Si2 C26 1.845(8) . ? Si2 C27 1.892(11) . ? Si2 C27 1.892(11) 7_565 ? C1 C2 1.401(7) 7_565 ? C1 C2 1.401(7) . ? C1 C13 1.433(11) . ? C2 C3 1.408(9) . ? C2 C11 1.433(7) . ? C3 C4 1.353(10) . ? C4 C5 1.433(10) . ? C4 C9 1.453(9) . ? C5 C6 1.324(12) . ? C6 C7 1.429(12) . ? C6 C37 1.55(2) . ? C7 C37' 1.24(6) . ? C7 C8 1.361(11) . ? C8 C9 1.427(10) . ? C9 C10 1.372(10) . ? C10 C11 1.395(9) . ? C11 C12 1.415(7) . ? C12 C11 1.415(7) 7_565 ? C12 C25 1.430(11) . ? C13 C14 1.197(12) . ? C15 C16 1.534(15) . ? C15 C19 1.531(12) . ? C16 C17 1.521(15) . ? C17 C18 1.537(15) . ? C18 C19 1.499(14) . ? C20 C21 1.514(9) . ? C20 C24 1.541(10) . ? C21 C22 1.527(11) . ? C22 C23 1.475(12) . ? C23 C24 1.525(11) . ? C25 C26 1.180(11) . ? C27 C28 1.519(14) . ? C27 C31 1.527(14) . ? C28 C29 1.518(16) . ? C29 C30 1.509(16) . ? C30 C31 1.507(15) . ? C32 C36 1.507(11) . ? C32 C33 1.520(11) . ? C33 C34 1.517(12) . ? C34 C35 1.507(14) . ? C35 C36 1.534(12) . ? C37 N1 1.40(2) . ? N1 C37 1.40(2) 7_575 ? C37' N1' 1.47(6) . ? N1' C37' 1.47(6) 7_575 ? 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 C15 Si1 C15 13.2(12) 7_565 . ? C15 Si1 C14 109.8(4) 7_565 . ? C15 Si1 C14 109.8(4) . . ? C15 Si1 C20 102.8(6) 7_565 . ? C15 Si1 C20 114.7(6) . . ? C14 Si1 C20 105.9(3) . . ? C15 Si1 C20 114.7(6) 7_565 7_565 ? C15 Si1 C20 102.8(6) . 7_565 ? C14 Si1 C20 105.9(3) . 7_565 ? C20 Si1 C20 117.2(5) . 7_565 ? C32 Si2 C32 109.8(5) 7_565 . ? C32 Si2 C26 108.5(3) 7_565 . ? C32 Si2 C26 108.5(3) . . ? C32 Si2 C27 105.6(5) 7_565 . ? C32 Si2 C27 118.2(5) . . ? C26 Si2 C27 105.9(4) . . ? C32 Si2 C27 118.2(5) 7_565 7_565 ? C32 Si2 C27 105.6(5) . 7_565 ? C26 Si2 C27 105.9(4) . 7_565 ? C27 Si2 C27 14.3(10) . 7_565 ? C2 C1 C2 121.7(7) 7_565 . ? C2 C1 C13 119.1(4) 7_565 . ? C2 C1 C13 119.1(4) . . ? C1 C2 C3 123.0(5) . . ? C1 C2 C11 119.4(6) . . ? C3 C2 C11 117.6(6) . . ? C4 C3 C2 123.1(6) . . ? C3 C4 C5 123.8(7) . . ? C3 C4 C9 118.9(7) . . ? C5 C4 C9 117.3(7) . . ? C6 C5 C4 122.9(8) . . ? C5 C6 C7 120.5(9) . . ? C5 C6 C37 110.3(10) . . ? C7 C6 C37 129.1(11) . . ? C37' C7 C8 119(2) . . ? C37' C7 C6 121(2) . . ? C8 C7 C6 119.4(9) . . ? C7 C8 C9 122.3(8) . . ? C10 C9 C8 123.4(7) . . ? C10 C9 C4 119.0(7) . . ? C8 C9 C4 117.6(7) . . ? C9 C10 C11 121.9(6) . . ? C10 C11 C12 121.3(5) . . ? C10 C11 C2 119.4(6) . . ? C12 C11 C2 119.2(6) . . ? C11 C12 C11 120.9(7) 7_565 . ? C11 C12 C25 119.6(4) 7_565 . ? C11 C12 C25 119.6(4) . . ? C14 C13 C1 176.9(9) . . ? C13 C14 Si1 179.1(8) . . ? C16 C15 C19 101.8(10) . . ? C16 C15 Si1 118.1(11) . . ? C19 C15 Si1 112.8(8) . . ? C15 C16 C17 103.2(10) . . ? C16 C17 C18 108.1(10) . . ? C19 C18 C17 104.2(10) . . ? C18 C19 C15 105.5(10) . . ? C21 C20 C24 103.3(6) . . ? C21 C20 Si1 116.1(6) . . ? C24 C20 Si1 114.8(5) . . ? C20 C21 C22 104.9(7) . . ? C23 C22 C21 103.2(7) . . ? C22 C23 C24 103.9(8) . . ? C23 C24 C20 107.6(7) . . ? C26 C25 C12 179.1(8) . . ? C25 C26 Si2 174.2(8) . . ? C28 C27 C31 104.9(9) . . ? C28 C27 Si2 118.0(10) . . ? C31 C27 Si2 110.4(11) . . ? C27 C28 C29 101.3(11) . . ? C30 C29 C28 106.3(12) . . ? C31 C30 C29 105.0(12) . . ? C30 C31 C27 107.1(11) . . ? C36 C32 C33 103.4(8) . . ? C36 C32 Si2 117.1(6) . . ? C33 C32 Si2 113.7(6) . . ? C32 C33 C34 101.8(9) . . ? C35 C34 C33 107.3(9) . . ? C34 C35 C36 104.3(9) . . ? C32 C36 C35 107.0(9) . . ? N1 C37 C6 165.7(16) . . ? C37 N1 C37 128.9(19) 7_575 . ? C7 C37' N1' 168(4) . . ? C37' N1' C37' 139(5) 7_575 . ? 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 C2 C1 C2 C3 175.3(4) 7_565 . . . ? C13 C1 C2 C3 -7.0(10) . . . . ? C2 C1 C2 C11 -3.3(10) 7_565 . . . ? C13 C1 C2 C11 174.4(6) . . . . ? C1 C2 C3 C4 179.9(6) . . . . ? C11 C2 C3 C4 -1.5(8) . . . . ? C2 C3 C4 C5 -179.2(6) . . . . ? C2 C3 C4 C9 -0.1(9) . . . . ? C3 C4 C5 C6 179.0(7) . . . . ? C9 C4 C5 C6 -0.1(10) . . . . ? C4 C5 C6 C7 0.1(11) . . . . ? C4 C5 C6 C37 -178.7(7) . . . . ? C5 C6 C7 C37' 175(2) . . . . ? C37 C6 C7 C37' -6(3) . . . . ? C5 C6 C7 C8 0.7(11) . . . . ? C37 C6 C7 C8 179.2(9) . . . . ? C37' C7 C8 C9 -176(2) . . . . ? C6 C7 C8 C9 -1.5(10) . . . . ? C7 C8 C9 C10 -178.9(6) . . . . ? C7 C8 C9 C4 1.4(9) . . . . ? C3 C4 C9 C10 0.5(8) . . . . ? C5 C4 C9 C10 179.7(5) . . . . ? C3 C4 C9 C8 -179.8(6) . . . . ? C5 C4 C9 C8 -0.6(8) . . . . ? C8 C9 C10 C11 -179.0(5) . . . . ? C4 C9 C10 C11 0.7(8) . . . . ? C9 C10 C11 C12 179.7(6) . . . . ? C9 C10 C11 C2 -2.3(8) . . . . ? C1 C2 C11 C10 -178.7(5) . . . . ? C3 C2 C11 C10 2.6(7) . . . . ? C1 C2 C11 C12 -0.6(8) . . . . ? C3 C2 C11 C12 -179.3(5) . . . . ? C10 C11 C12 C11 -177.5(4) . . . 7_565 ? C2 C11 C12 C11 4.5(10) . . . 7_565 ? C10 C11 C12 C25 2.5(9) . . . . ? C2 C11 C12 C25 -175.5(6) . . . . ? C2 C1 C13 C14 88.9(6) 7_565 . . . ? C2 C1 C13 C14 -88.9(6) . . . . ? C1 C13 C14 Si1 0.00(14) . . . . ? C15 Si1 C14 C13 7.0(6) 7_565 . . . ? C15 Si1 C14 C13 -7.0(6) . . . . ? C20 Si1 C14 C13 117.4(3) . . . . ? C20 Si1 C14 C13 -117.4(3) 7_565 . . . ? C15 Si1 C15 C16 -17.8(11) 7_565 . . . ? C14 Si1 C15 C16 74.6(12) . . . . ? C20 Si1 C15 C16 -44.5(12) . . . . ? C20 Si1 C15 C16 -173.0(11) 7_565 . . . ? C15 Si1 C15 C19 100.6(12) 7_565 . . . ? C14 Si1 C15 C19 -167.1(10) . . . . ? C20 Si1 C15 C19 73.8(13) . . . . ? C20 Si1 C15 C19 -54.6(13) 7_565 . . . ? C19 C15 C16 C17 37.7(16) . . . . ? Si1 C15 C16 C17 161.7(11) . . . . ? C15 C16 C17 C18 -21.5(18) . . . . ? C16 C17 C18 C19 -3.7(17) . . . . ? C17 C18 C19 C15 27.9(16) . . . . ? C16 C15 C19 C18 -41.4(15) . . . . ? Si1 C15 C19 C18 -168.9(11) . . . . ? C15 Si1 C20 C21 -178.6(6) 7_565 . . . ? C15 Si1 C20 C21 -172.6(6) . . . . ? C14 Si1 C20 C21 66.1(6) . . . . ? C20 Si1 C20 C21 -51.8(7) 7_565 . . . ? C15 Si1 C20 C24 60.7(7) 7_565 . . . ? C15 Si1 C20 C24 66.8(7) . . . . ? C14 Si1 C20 C24 -54.5(6) . . . . ? C20 Si1 C20 C24 -172.4(4) 7_565 . . . ? C24 C20 C21 C22 -26.5(8) . . . . ? Si1 C20 C21 C22 -153.1(6) . . . . ? C20 C21 C22 C23 41.4(9) . . . . ? C21 C22 C23 C24 -38.4(11) . . . . ? C22 C23 C24 C20 22.2(11) . . . . ? C21 C20 C24 C23 3.1(9) . . . . ? Si1 C20 C24 C23 130.6(7) . . . . ? C11 C12 C25 C26 -90.0(6) 7_565 . . . ? C11 C12 C25 C26 90.0(6) . . . . ? C12 C25 C26 Si2 0.00(10) . . . . ? C32 Si2 C26 C25 120.4(3) 7_565 . . . ? C32 Si2 C26 C25 -120.4(3) . . . . ? C27 Si2 C26 C25 7.4(5) . . . . ? C27 Si2 C26 C25 -7.4(5) 7_565 . . . ? C32 Si2 C27 C28 -57.8(13) 7_565 . . . ? C32 Si2 C27 C28 178.9(11) . . . . ? C26 Si2 C27 C28 57.2(13) . . . . ? C27 Si2 C27 C28 149.2(12) 7_565 . . . ? C32 Si2 C27 C31 -178.4(11) 7_565 . . . ? C32 Si2 C27 C31 58.4(12) . . . . ? C26 Si2 C27 C31 -63.4(12) . . . . ? C27 Si2 C27 C31 28.6(12) 7_565 . . . ? C31 C27 C28 C29 -36.2(14) . . . . ? Si2 C27 C28 C29 -159.7(11) . . . . ? C27 C28 C29 C30 39(2) . . . . ? C28 C29 C30 C31 -26(3) . . . . ? C29 C30 C31 C27 3(2) . . . . ? C28 C27 C31 C30 21.4(16) . . . . ? Si2 C27 C31 C30 149.5(14) . . . . ? C32 Si2 C32 C36 179.2(5) 7_565 . . . ? C26 Si2 C32 C36 60.9(8) . . . . ? C27 Si2 C32 C36 -59.6(9) . . . . ? C27 Si2 C32 C36 -52.3(8) 7_565 . . . ? C32 Si2 C32 C33 58.7(9) 7_565 . . . ? C26 Si2 C32 C33 -59.7(8) . . . . ? C27 Si2 C32 C33 179.8(7) . . . . ? C27 Si2 C32 C33 -172.8(7) 7_565 . . . ? C36 C32 C33 C34 39.9(10) . . . . ? Si2 C32 C33 C34 167.9(8) . . . . ? C32 C33 C34 C35 -35.4(14) . . . . ? C33 C34 C35 C36 16.7(15) . . . . ? C33 C32 C36 C35 -30.6(11) . . . . ? Si2 C32 C36 C35 -156.4(8) . . . . ? C34 C35 C36 C32 8.7(14) . . . . ? C5 C6 C37 N1 -177(5) . . . . ? C7 C6 C37 N1 4(6) . . . . ? C6 C37 N1 C37 -6(7) . . . 7_575 ? C8 C7 C37' N1' 166(18) . . . . ? C6 C7 C37' N1' -9(21) . . . . ? C7 C37' N1' C37' 31(25) . . . 7_575 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 69.04 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.589 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.084 # Attachment 'k07415 _ DicyanoTCPS.cif' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # If this CIF has been generated directly or indirectly from an entry in the # Cambridge Structural Database, then it will include bibliographic, chemical, # crystal, experimental, refinement or atomic coordinate data resulting from # the CCDC's data processing and validation procedures. Files generated from # CSD entries are Copyright 2007 Cambridge Crystallographic Data Centre. They # may be used in bona fide research applications only, and may not be copied or # further disseminated in any form, whether machine-readable or not, except for # the purposes of generating routine backup copies on your local computer # system. # # Files arising from any other source may also contain material that is the # copyright of third parties, including the originator, and you should check # with the originator concerning the permitted uses of the information # contained in this CIF. # # For further information on the CCDC and the free tools enCIFer and Mercury # for validating and visualising CIF files, please visit www.ccdc.cam.ac.uk # ####################################################################### data_CompoundX _database_code_depnum_ccdc_archive 'CCDC 722604' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,-y,1/2+z 3 1/2+x,1/2-y,1/2-z 4 -x,1/2+y,-z 5 -x,-y,-z 6 1/2+x,y,1/2-z 7 1/2-x,1/2+y,1/2+z 8 x,1/2-y,z _cell_length_a 16.5590(1) _cell_length_b 17.6140(1) _cell_length_c 16.5780(2) _cell_angle_alpha 90.0000(4) _cell_angle_beta 90.0000(3) _cell_angle_gamma 90.0000(4) _cell_volume 4835.31 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z SI1 Si 0.34252 0.25 0.68005 SI2 Si -0.22768 0.25 0.25868 C3 C 0.04288 0.17916 0.41516 C4 C -0.12655 0.25 0.30816 C5 C 0.26421 0.25 0.59907 C6 C 0.1448 0.25 0.49528 C7 C 0.11691 0.04172 0.46318 C8 C -0.0653 0.25 0.34452 C9 C 0.12215 -0.096 0.45566 C10 C 0.11268 0.17974 0.46828 C11 C 0.00687 0.25 0.39259 C12 C 0.01637 -0.02868 0.38137 C13 C -0.23402 0.3398 0.1998 C14 C 0.14651 0.1103 0.49143 C15 C 0.21111 0.25 0.55085 C16 C 0.0473 0.04153 0.40908 C17 C 0.01232 0.10949 0.38789 C18 C 0.153 -0.02913 0.48516 C19 C 0.28478 0.25 0.77611 C20 C 0.40529 0.16267 0.66797 C21 C -0.17224 0.34797 0.12908 C22 C -0.30776 0.25 0.33911 C23 C -0.15678 0.43207 0.11841 C24 C 0.05316 -0.09693 0.40287 C25 C -0.21701 0.41301 0.25054 C26 C 0.44648 0.15351 0.58392 C27 C 0.16782 0.3096 0.85105 N28 N -0.0087 -0.21622 0.35151 C29 C 0.47952 0.07317 0.58412 N30 N 0.18954 -0.21672 0.49037 C31 C 0.01691 -0.15964 0.37708 C32 C 0.15833 -0.15955 0.47561 C33 C 0.22839 0.31868 0.78714 C34 C 0.36433 0.08713 0.6793 C37 C -0.15135 0.45773 0.20429 C38 C 0.4219 0.02955 0.62595 C41 C -0.40426 0.207 0.43284 C42 C -0.32396 0.18478 0.38402 C3A C 0.04288 0.32085 0.41515 C7A C 0.11691 0.45827 0.46318 C9A C 0.12215 0.596 0.45566 C10A C 0.11269 0.32026 0.46828 C12A C 0.01637 0.52868 0.38137 C13A C -0.23402 0.1602 0.1998 C14A C 0.14651 0.38969 0.49143 C16A C 0.04729 0.45847 0.40908 C17A C 0.01232 0.39051 0.38789 C18A C 0.153 0.52913 0.48515 C20A C 0.40529 0.33733 0.66798 C21A C -0.17224 0.15203 0.12908 C23A C -0.15678 0.06793 0.11841 C24A C 0.05316 0.59693 0.40286 C25A C -0.217 0.08699 0.25053 C26A C 0.44648 0.34649 0.58392 C29A C 0.47952 0.42683 0.58411 C33A C 0.22839 0.18132 0.78713 C34A C 0.36433 0.41287 0.6793 C37A C -0.15135 0.04227 0.20429 C38A C 0.42191 0.47044 0.62595 C41A C -0.40427 0.293 0.43284 C42A C -0.32396 0.31522 0.38402 C999 C 0.15847 0.2202 0.8437 #END # Attachment 'k08034x_DicyanoTCHS.cif' data_k08034x _database_code_depnum_ccdc_archive 'CCDC 722605' _vrf_THETM01_k08034x ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Yes the resolution is on the low side. We do not waste resources collecting noise. ; _vrf_PLAT023_k08034x ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 22.50 Deg. RESPONSE: This squawk is essentially the same as the previous one - please see above response. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H74 N2 Si2' _chemical_formula_sum 'C64 H74 N2 Si2' _chemical_formula_weight 927.43 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 16.6409(6) _cell_length_b 17.5827(7) _cell_length_c 18.8903(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5527.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used 5567 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'cut block' _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.115 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.974 _exptl_absorpt_correction_T_max 0.985 _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 44723 _diffrn_reflns_av_R_equivalents 0.106 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3748 _reflns_number_gt 2122 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 2008)' _computing_publication_material ; SHELX97-2 (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 C-H distances of 0.99 \%A (R~2~CH~2~), 1.00 \%A (R~3~CH) and 0.95 \%A (C~Ar~H) with U~iso~(H) values set to 1.2U~eq~ of the attached C atom. Important notice: Due to the nature of disorder in this crystal structure it would be a bad idea to make any bold claims with regard to *molecular* structure in a publication. The quality is such that the atom connectivity is well enough established, and the gross geometry is fine, but any unusual bond lengths, angles or atomic displacement parameters are merely a consequence of the disorder. The molecule is modelled as disordered across a mirror plane, but this is really a compromise. The relative positioning of the pentacene ring systems is largely ok, and thus the packing is established, but the structure is not "good" in the normal sense. ; _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^)+(0.0313P)^2^+15.3078P] 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 3748 _refine_ls_number_parameters 391 _refine_ls_number_restraints 76 _refine_ls_R_factor_all 0.1571 _refine_ls_R_factor_gt 0.0891 _refine_ls_wR_factor_ref 0.2075 _refine_ls_wR_factor_gt 0.1833 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.109 _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 0.85150(14) 0.2500 0.68190(13) 0.0560(7) Uani 1 2 d S . . Si2 Si 0.40155(15) 0.2500 0.20739(13) 0.0558(7) Uani 1 2 d S . . C1 C 0.6563(5) 0.2500 0.5221(4) 0.063(3) Uani 1 2 d S . . C2 C 0.6284(4) 0.1796(4) 0.4945(3) 0.0604(18) Uani 1 1 d . . . C3 C 0.6517(4) 0.1110(5) 0.5236(3) 0.076(2) Uani 1 1 d . . . H3 H 0.6859 0.1114 0.5638 0.092 Uiso 1 1 calc R . . C4 C 0.6271(5) 0.0420(5) 0.4964(3) 0.087(3) Uani 1 1 d . . . C5 C 0.6508(5) -0.0303(5) 0.5254(4) 0.095(3) Uani 1 1 d . . . H5 H 0.6847 -0.0312 0.5658 0.114 Uiso 1 1 calc R . . C6 C 0.6263(5) -0.0967(5) 0.4971(4) 0.095(2) Uani 1 1 d U . . C7 C 0.5721(5) -0.0984(5) 0.4375(4) 0.093(2) Uani 1 1 d U . . C8 C 0.5472(5) -0.0292(4) 0.4088(4) 0.087(2) Uani 1 1 d . . . H8 H 0.5120 -0.0296 0.3692 0.105 Uiso 1 1 calc R . . C9 C 0.5725(4) 0.0415(4) 0.4365(3) 0.075(2) Uani 1 1 d . . . C10 C 0.5494(4) 0.1104(4) 0.4073(3) 0.068(2) Uani 1 1 d . . . H10 H 0.5147 0.1102 0.3674 0.081 Uiso 1 1 calc R . . C11 C 0.5751(4) 0.1801(4) 0.4344(3) 0.0574(17) Uani 1 1 d . . . C12 C 0.5515(5) 0.2500 0.4049(4) 0.052(2) Uani 1 2 d S . . C13 C 0.7136(6) 0.2500 0.5777(5) 0.071(3) Uani 1 2 d S . . C14 C 0.7660(6) 0.2500 0.6227(5) 0.070(3) Uani 1 2 d S A . C15 C 0.8944(10) 0.1476(10) 0.6544(9) 0.066(7) Uani 0.50 1 d PD A 1 H15 H 0.8503 0.1096 0.6607 0.079 Uiso 0.50 1 calc PR A 1 C16 C 0.9644(9) 0.1226(8) 0.6982(8) 0.063(5) Uani 0.50 1 d PD A 1 H16A H 0.9475 0.1197 0.7484 0.076 Uiso 0.50 1 calc PR A 1 H16B H 1.0075 0.1611 0.6947 0.076 Uiso 0.50 1 calc PR A 1 C17 C 0.9976(13) 0.0459(12) 0.6757(9) 0.083(9) Uani 0.50 1 d PD A 1 H17A H 1.0467 0.0344 0.7033 0.100 Uiso 0.50 1 calc PR A 1 H17B H 0.9575 0.0057 0.6858 0.100 Uiso 0.50 1 calc PR A 1 C18 C 1.0172(9) 0.0460(8) 0.5982(8) 0.082(5) Uani 0.50 1 d PD A 1 H18A H 1.0355 -0.0054 0.5841 0.098 Uiso 0.50 1 calc PR A 1 H18B H 1.0619 0.0820 0.5894 0.098 Uiso 0.50 1 calc PR A 1 C19 C 0.9440(9) 0.0689(9) 0.5521(9) 0.090(6) Uani 0.50 1 d PD A 1 H19A H 0.9590 0.0695 0.5014 0.109 Uiso 0.50 1 calc PR A 1 H19B H 0.8994 0.0323 0.5588 0.109 Uiso 0.50 1 calc PR A 1 C20 C 0.9185(8) 0.1478(8) 0.5759(7) 0.067(4) Uani 0.50 1 d PD A 1 H20A H 0.8724 0.1651 0.5469 0.081 Uiso 0.50 1 calc PR A 1 H20B H 0.9633 0.1840 0.5686 0.081 Uiso 0.50 1 calc PR A 1 C15' C 0.9231(10) 0.1735(9) 0.6661(9) 0.050(5) Uani 0.50 1 d PD A 2 H15' H 0.9606 0.1953 0.6301 0.060 Uiso 0.50 1 calc PR A 2 C16' C 0.9763(8) 0.1557(7) 0.7270(8) 0.054(5) Uani 0.50 1 d PD A 2 H16C H 0.9425 0.1414 0.7680 0.064 Uiso 0.50 1 calc PR A 2 H16D H 1.0065 0.2021 0.7400 0.064 Uiso 0.50 1 calc PR A 2 C17' C 1.0355(9) 0.0923(8) 0.7128(9) 0.089(5) Uani 0.50 1 d PD A 2 H17C H 1.0790 0.1117 0.6820 0.107 Uiso 0.50 1 calc PR A 2 H17D H 1.0601 0.0763 0.7582 0.107 Uiso 0.50 1 calc PR A 2 C18' C 0.9979(19) 0.0253(13) 0.6786(17) 0.17(2) Uani 0.50 1 d PD A 2 H18C H 0.9626 0.0000 0.7136 0.202 Uiso 0.50 1 calc PR A 2 H18D H 1.0408 -0.0112 0.6658 0.202 Uiso 0.50 1 calc PR A 2 C19' C 0.9484(11) 0.0426(10) 0.6123(12) 0.111(7) Uani 0.50 1 d PD A 2 H19C H 0.9843 0.0595 0.5735 0.133 Uiso 0.50 1 calc PR A 2 H19D H 0.9199 -0.0039 0.5965 0.133 Uiso 0.50 1 calc PR A 2 C20' C 0.8878(10) 0.1048(9) 0.6293(14) 0.117(10) Uani 0.50 1 d PD A 2 H20C H 0.8622 0.1217 0.5846 0.140 Uiso 0.50 1 calc PR A 2 H20D H 0.8451 0.0831 0.6597 0.140 Uiso 0.50 1 calc PR A 2 C21 C 0.8096(5) 0.2500 0.7726(5) 0.069(3) Uani 1 2 d S . . H21 H 0.8562 0.2500 0.8061 0.083 Uiso 1 2 calc SR . . C22 C 0.7599(4) 0.1802(4) 0.7891(4) 0.091(2) Uani 1 1 d . . . H22A H 0.7945 0.1346 0.7846 0.110 Uiso 1 1 calc R A . H22B H 0.7165 0.1758 0.7535 0.110 Uiso 1 1 calc R . . C23 C 0.7225(5) 0.1808(6) 0.8624(5) 0.139(4) Uani 1 1 d . A . H23A H 0.6901 0.1341 0.8691 0.166 Uiso 1 1 calc R . . H23B H 0.7655 0.1811 0.8986 0.166 Uiso 1 1 calc R . . C24 C 0.6697(7) 0.2500 0.8718(6) 0.111(4) Uani 1 2 d S . . H24A H 0.6452 0.2500 0.9195 0.133 Uiso 1 2 calc SR A . H24B H 0.6261 0.2500 0.8361 0.133 Uiso 1 2 calc SR . . C25 C 0.5022(5) 0.2500 0.3420(5) 0.059(2) Uani 1 2 d S . . C26 C 0.4630(5) 0.2500 0.2878(5) 0.051(2) Uani 1 2 d S . . C27 C 0.3437(4) 0.1570(3) 0.2113(3) 0.0621(18) Uani 1 1 d D . . H27 H 0.3855 0.1165 0.2168 0.074 Uiso 1 1 calc R . . C28 C 0.2892(4) 0.1489(3) 0.2758(3) 0.0651(19) Uani 1 1 d D . . H28A H 0.2451 0.1865 0.2726 0.078 Uiso 1 1 calc R . . H28B H 0.3205 0.1601 0.3191 0.078 Uiso 1 1 calc R . . C29 C 0.2534(4) 0.0691(4) 0.2817(3) 0.073(2) Uani 1 1 d D . . H29A H 0.2968 0.0316 0.2901 0.088 Uiso 1 1 calc R . . H29B H 0.2158 0.0670 0.3223 0.088 Uiso 1 1 calc R . . C30 C 0.2097(4) 0.0496(4) 0.2152(3) 0.085(2) Uani 1 1 d D . . H30A H 0.1631 0.0841 0.2097 0.101 Uiso 1 1 calc R . . H30B H 0.1890 -0.0031 0.2187 0.101 Uiso 1 1 calc R . . C31 C 0.2634(5) 0.0561(5) 0.1502(4) 0.103(3) Uani 1 1 d D . . H31A H 0.2318 0.0442 0.1073 0.123 Uiso 1 1 calc R . . H31B H 0.3077 0.0187 0.1537 0.123 Uiso 1 1 calc R . . C32 C 0.2988(4) 0.1369(4) 0.1438(3) 0.089(2) Uani 1 1 d D . . H32A H 0.3359 0.1392 0.1029 0.107 Uiso 1 1 calc R . . H32B H 0.2549 0.1740 0.1357 0.107 Uiso 1 1 calc R . . C33 C 0.4737(5) 0.2500 0.1310(4) 0.058(2) Uani 1 2 d S . . H33 H 0.4414 0.2500 0.0863 0.069 Uiso 1 2 calc SR . . C34 C 0.5272(4) 0.1798(4) 0.1302(4) 0.090(2) Uani 1 1 d . . . H34A H 0.4929 0.1341 0.1248 0.108 Uiso 1 1 calc R . . H34B H 0.5550 0.1758 0.1764 0.108 Uiso 1 1 calc R . . C35 C 0.5901(5) 0.1801(5) 0.0711(4) 0.103(3) Uani 1 1 d . . . H35A H 0.6252 0.1350 0.0760 0.124 Uiso 1 1 calc R . . H35B H 0.5628 0.1771 0.0247 0.124 Uiso 1 1 calc R . . C36 C 0.6398(7) 0.2500 0.0739(6) 0.121(5) Uani 1 2 d S . . H36A H 0.6717 0.2500 0.1181 0.145 Uiso 1 2 calc SR . . H36B H 0.6777 0.2500 0.0335 0.145 Uiso 1 2 calc SR . . C37 C 0.6373(8) -0.1756(8) 0.5265(6) 0.073(3) Uani 0.50 1 d PDU . . N1 N 0.6555(5) -0.2500 0.5485(4) 0.097(3) Uani 1 2 d SDU . . C38 C 0.5292(8) -0.1748(8) 0.4070(7) 0.083(3) Uani 0.50 1 d PDU . . N2 N 0.5069(5) -0.2500 0.3843(5) 0.105(3) Uani 1 2 d SDU . . 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 0.0464(14) 0.0630(18) 0.0587(15) 0.000 -0.0064(12) 0.000 Si2 0.0526(15) 0.0567(17) 0.0581(15) 0.000 -0.0096(13) 0.000 C1 0.052(6) 0.095(9) 0.041(5) 0.000 0.007(5) 0.000 C2 0.056(4) 0.076(5) 0.050(4) -0.006(4) -0.005(3) 0.021(4) C3 0.083(5) 0.091(6) 0.056(4) -0.012(5) -0.003(4) 0.044(5) C4 0.119(7) 0.086(6) 0.055(4) -0.013(5) -0.005(4) 0.063(6) C5 0.132(7) 0.091(6) 0.063(5) -0.014(5) -0.011(5) 0.069(6) C6 0.128(6) 0.090(5) 0.066(4) -0.009(4) 0.014(4) 0.048(5) C7 0.127(6) 0.088(5) 0.062(4) -0.010(4) 0.014(4) 0.046(4) C8 0.135(7) 0.067(6) 0.059(4) -0.013(4) 0.001(4) 0.038(5) C9 0.106(6) 0.067(6) 0.052(4) -0.015(4) -0.006(4) 0.037(5) C10 0.075(5) 0.074(6) 0.054(4) -0.011(4) -0.009(4) 0.027(4) C11 0.064(4) 0.059(5) 0.050(4) -0.006(4) -0.003(3) 0.012(4) C12 0.039(5) 0.074(8) 0.045(5) 0.000 0.002(4) 0.000 C13 0.054(6) 0.106(9) 0.053(6) 0.000 0.005(5) 0.000 C14 0.060(6) 0.091(8) 0.059(6) 0.000 0.000(5) 0.000 C15 0.046(11) 0.033(17) 0.119(17) 0.010(13) -0.013(10) -0.016(11) C16 0.063(11) 0.033(11) 0.093(13) -0.006(10) -0.002(9) -0.024(10) C17 0.050(15) 0.051(16) 0.15(2) -0.009(13) 0.032(17) 0.009(11) C18 0.070(11) 0.040(10) 0.136(15) 0.012(10) 0.034(11) -0.004(9) C19 0.068(11) 0.093(15) 0.110(13) -0.030(12) 0.000(11) 0.003(10) C20 0.059(9) 0.062(11) 0.081(10) -0.015(9) -0.006(8) 0.011(8) C15' 0.072(14) 0.014(9) 0.063(9) -0.008(7) 0.009(9) -0.001(10) C16' 0.030(8) 0.028(10) 0.103(13) 0.001(9) -0.016(7) -0.001(7) C17' 0.067(11) 0.058(12) 0.142(15) 0.001(11) 0.005(11) 0.017(10) C18' 0.11(3) 0.029(14) 0.37(6) 0.01(2) -0.02(3) 0.010(14) C19' 0.088(15) 0.071(15) 0.17(2) -0.046(16) 0.002(17) 0.011(13) C20' 0.068(12) 0.051(15) 0.23(3) -0.049(16) -0.012(14) 0.009(12) C21 0.048(6) 0.089(8) 0.069(6) 0.000 -0.010(5) 0.000 C22 0.078(5) 0.083(6) 0.114(6) 0.032(5) 0.035(5) 0.021(5) C23 0.082(6) 0.199(11) 0.135(8) 0.083(8) 0.038(6) 0.039(7) C24 0.074(8) 0.182(14) 0.077(8) 0.000 0.014(6) 0.000 C25 0.056(6) 0.069(7) 0.052(6) 0.000 0.002(5) 0.000 C26 0.056(6) 0.036(5) 0.061(6) 0.000 0.000(5) 0.000 C27 0.059(4) 0.061(5) 0.066(4) -0.007(3) -0.007(4) -0.004(3) C28 0.068(4) 0.055(5) 0.072(4) 0.001(4) -0.007(4) -0.010(4) C29 0.080(5) 0.060(5) 0.080(5) 0.002(4) -0.005(4) -0.010(4) C30 0.085(5) 0.079(6) 0.090(5) -0.008(5) -0.001(5) -0.026(4) C31 0.091(6) 0.130(8) 0.087(5) -0.038(5) 0.002(5) -0.042(6) C32 0.083(5) 0.118(7) 0.067(5) -0.014(5) -0.010(4) -0.041(5) C33 0.063(6) 0.053(6) 0.057(5) 0.000 -0.009(5) 0.000 C34 0.100(6) 0.090(6) 0.080(5) 0.003(5) 0.027(5) 0.023(5) C35 0.103(7) 0.115(8) 0.092(6) 0.016(6) 0.019(5) 0.041(6) C36 0.058(8) 0.239(19) 0.066(7) 0.000 0.003(6) 0.000 C37 0.082(6) 0.082(6) 0.055(6) -0.014(5) 0.010(5) 0.012(6) N1 0.089(6) 0.118(6) 0.084(5) 0.000 0.009(5) 0.000 C38 0.081(7) 0.099(7) 0.068(6) 0.006(5) 0.026(5) 0.032(6) N2 0.086(6) 0.141(7) 0.089(6) 0.000 0.014(5) 0.000 _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 C14 1.810(10) . ? Si1 C15' 1.821(15) 8_565 ? Si1 C15' 1.821(15) . ? Si1 C21 1.850(9) . ? Si1 C15 2.005(17) 8_565 ? Si1 C15 2.005(17) . ? Si2 C26 1.831(9) . ? Si2 C33 1.878(9) . ? Si2 C27 1.899(6) . ? Si2 C27 1.900(6) 8_565 ? C1 C13 1.419(12) . ? C1 C2 1.422(7) 8_565 ? C1 C2 1.422(7) . ? C2 C3 1.380(9) . ? C2 C11 1.441(8) . ? C3 C4 1.380(9) . ? C3 H3 0.9500 . ? C4 C5 1.439(9) . ? C4 C9 1.451(9) . ? C5 C6 1.348(10) . ? C5 H5 0.9500 . ? C6 C7 1.443(10) . ? C6 C37 1.505(14) . ? C7 C8 1.393(9) . ? C7 C38 1.626(15) . ? C8 C9 1.413(9) . ? C8 H8 0.9500 . ? C9 C10 1.387(8) . ? C10 C11 1.394(8) . ? C10 H10 0.9500 . ? C11 C12 1.406(7) . ? C12 C11 1.406(7) 8_565 ? C12 C25 1.443(12) . ? C13 C14 1.216(11) . ? C15 C16 1.494(15) . ? C15 C20 1.536(15) . ? C15 H15 1.0000 . ? C16 C17 1.518(16) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.500(16) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.551(16) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.519(14) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C15' C16' 1.484(14) . ? C15' C20' 1.513(15) . ? C15' H15' 1.0000 . ? C16' C17' 1.512(14) . ? C16' H16C 0.9900 . ? C16' H16D 0.9900 . ? C17' C18' 1.482(18) . ? C17' H17C 0.9900 . ? C17' H17D 0.9900 . ? C18' C19' 1.531(19) . ? C18' H18C 0.9900 . ? C18' H18D 0.9900 . ? C19' C20' 1.523(15) . ? C19' H19C 0.9900 . ? C19' H19D 0.9900 . ? C20' H20C 0.9900 . ? C20' H20D 0.9900 . ? C21 C22 1.513(8) 8_565 ? C21 C22 1.513(8) . ? C21 H21 1.0000 . ? C22 C23 1.518(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.512(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C23 1.512(9) 8_565 ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.214(10) . ? C27 C32 1.521(7) . ? C27 C28 1.525(7) . ? C27 H27 1.0000 . ? C28 C29 1.528(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.492(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.522(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.542(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.522(8) 8_565 ? C33 C34 1.522(8) . ? C33 H33 1.0000 . ? C34 C35 1.530(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.482(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C35 1.482(9) 8_565 ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 N1 1.406(13) . ? N1 C37 1.406(13) 8 ? C38 N2 1.439(14) . ? N2 C38 1.439(14) 8 ? 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 C14 Si1 C15' 114.4(5) . 8_565 ? C14 Si1 C15' 114.4(5) . . ? C15' Si1 C15' 95.2(11) 8_565 . ? C14 Si1 C21 106.0(4) . . ? C15' Si1 C21 113.5(6) 8_565 . ? C15' Si1 C21 113.5(6) . . ? C14 Si1 C15 96.9(5) . 8_565 ? C15' Si1 C15 112.8(8) . 8_565 ? C21 Si1 C15 112.0(5) . 8_565 ? C14 Si1 C15 96.9(5) . . ? C15' Si1 C15 112.8(8) 8_565 . ? C21 Si1 C15 112.0(5) . . ? C15 Si1 C15 127.7(10) 8_565 . ? C26 Si2 C33 106.3(4) . . ? C26 Si2 C27 104.5(2) . . ? C33 Si2 C27 110.8(2) . . ? C26 Si2 C27 104.5(2) . 8_565 ? C33 Si2 C27 110.8(2) . 8_565 ? C27 Si2 C27 118.9(4) . 8_565 ? C13 C1 C2 119.4(4) . 8_565 ? C13 C1 C2 119.4(4) . . ? C2 C1 C2 121.1(8) 8_565 . ? C3 C2 C1 121.5(6) . . ? C3 C2 C11 119.4(6) . . ? C1 C2 C11 119.0(7) . . ? C4 C3 C2 122.5(6) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 123.7(7) . . ? C3 C4 C9 118.7(7) . . ? C5 C4 C9 117.6(8) . . ? C6 C5 C4 122.1(7) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 121.1(7) . . ? C5 C6 C37 127.9(8) . . ? C7 C6 C37 110.2(9) . . ? C8 C7 C6 118.1(8) . . ? C8 C7 C38 116.9(8) . . ? C6 C7 C38 124.6(8) . . ? C7 C8 C9 122.4(7) . . ? C7 C8 H8 118.8 . . ? C9 C8 H8 118.8 . . ? C10 C9 C8 122.6(7) . . ? C10 C9 C4 118.6(7) . . ? C8 C9 C4 118.7(7) . . ? C9 C10 C11 122.5(6) . . ? C9 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C10 C11 C12 122.5(6) . . ? C10 C11 C2 118.2(6) . . ? C12 C11 C2 119.3(7) . . ? C11 C12 C11 122.0(8) 8_565 . ? C11 C12 C25 119.0(4) 8_565 . ? C11 C12 C25 119.0(4) . . ? C14 C13 C1 176.5(9) . . ? C13 C14 Si1 173.9(8) . . ? C16 C15 C20 109.4(12) . . ? C16 C15 Si1 113.5(12) . . ? C20 C15 Si1 109.9(10) . . ? C16 C15 H15 107.9 . . ? C20 C15 H15 107.9 . . ? Si1 C15 H15 107.9 . . ? C15 C16 C17 113.0(13) . . ? 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 . . ? C18 C17 C16 110.6(15) . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? C17 C18 C19 112.2(14) . . ? C17 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? C17 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C20 C19 C18 106.9(11) . . ? C20 C19 H19A 110.3 . . ? C18 C19 H19A 110.3 . . ? C20 C19 H19B 110.3 . . ? C18 C19 H19B 110.3 . . ? H19A C19 H19B 108.6 . . ? C19 C20 C15 110.8(13) . . ? C19 C20 H20A 109.5 . . ? C15 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? C16' C15' C20' 114.8(15) . . ? C16' C15' Si1 114.8(10) . . ? C20' C15' Si1 114.3(11) . . ? C16' C15' H15' 103.7 . . ? C20' C15' H15' 103.7 . . ? Si1 C15' H15' 103.7 . . ? C15' C16' C17' 114.1(12) . . ? C15' C16' H16C 108.7 . . ? C17' C16' H16C 108.7 . . ? C15' C16' H16D 108.7 . . ? C17' C16' H16D 108.7 . . ? H16C C16' H16D 107.6 . . ? C18' C17' C16' 112.8(15) . . ? C18' C17' H17C 109.0 . . ? C16' C17' H17C 109.0 . . ? C18' C17' H17D 109.0 . . ? C16' C17' H17D 109.0 . . ? H17C C17' H17D 107.8 . . ? C17' C18' C19' 115.3(19) . . ? C17' C18' H18C 108.5 . . ? C19' C18' H18C 108.5 . . ? C17' C18' H18D 108.5 . . ? C19' C18' H18D 108.5 . . ? H18C C18' H18D 107.5 . . ? C20' C19' C18' 109.0(16) . . ? C20' C19' H19C 109.9 . . ? C18' C19' H19C 109.9 . . ? C20' C19' H19D 109.9 . . ? C18' C19' H19D 109.9 . . ? H19C C19' H19D 108.3 . . ? C15' C20' C19' 114.4(14) . . ? C15' C20' H20C 108.6 . . ? C19' C20' H20C 108.6 . . ? C15' C20' H20D 108.6 . . ? C19' C20' H20D 108.6 . . ? H20C C20' H20D 107.6 . . ? C22 C21 C22 108.5(8) 8_565 . ? C22 C21 Si1 113.4(5) 8_565 . ? C22 C21 Si1 113.4(5) . . ? C22 C21 H21 107.1 8_565 . ? C22 C21 H21 107.1 . . ? Si1 C21 H21 107.1 . . ? C21 C22 C23 114.0(8) . . ? C21 C22 H22A 108.8 . . ? C23 C22 H22A 108.8 . . ? C21 C22 H22B 108.8 . . ? C23 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C22 110.5(7) . . ? C24 C23 H23A 109.5 . . ? C22 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? C23 C24 C23 107.2(10) . 8_565 ? C23 C24 H24A 110.3 . . ? C23 C24 H24A 110.3 8_565 . ? C23 C24 H24B 110.3 . . ? C23 C24 H24B 110.3 8_565 . ? H24A C24 H24B 108.5 . . ? C26 C25 C12 177.9(9) . . ? C25 C26 Si2 178.6(8) . . ? C32 C27 C28 110.9(5) . . ? C32 C27 Si2 114.6(4) . . ? C28 C27 Si2 114.4(4) . . ? C32 C27 H27 105.3 . . ? C28 C27 H27 105.3 . . ? Si2 C27 H27 105.3 . . ? C27 C28 C29 112.1(5) . . ? C27 C28 H28A 109.2 . . ? C29 C28 H28A 109.2 . . ? C27 C28 H28B 109.2 . . ? C29 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C30 C29 C28 109.8(5) . . ? C30 C29 H29A 109.7 . . ? C28 C29 H29A 109.7 . . ? C30 C29 H29B 109.7 . . ? C28 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C29 C30 C31 112.1(6) . . ? C29 C30 H30A 109.2 . . ? C31 C30 H30A 109.2 . . ? C29 C30 H30B 109.2 . . ? C31 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C30 C31 C32 111.0(6) . . ? C30 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? C30 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C27 C32 C31 109.5(6) . . ? C27 C32 H32A 109.8 . . ? C31 C32 H32A 109.8 . . ? C27 C32 H32B 109.8 . . ? C31 C32 H32B 109.8 . . ? H32A C32 H32B 108.2 . . ? C34 C33 C34 108.4(8) 8_565 . ? C34 C33 Si2 112.4(4) 8_565 . ? C34 C33 Si2 112.4(4) . . ? C34 C33 H33 107.8 8_565 . ? C34 C33 H33 107.8 . . ? Si2 C33 H33 107.8 . . ? C33 C34 C35 113.8(6) . . ? C33 C34 H34A 108.8 . . ? C35 C34 H34A 108.8 . . ? C33 C34 H34B 108.8 . . ? C35 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? C36 C35 C34 111.1(8) . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35B 109.4 . . ? C34 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C35 112.0(10) 8_565 . ? C35 C36 H36A 109.2 8_565 . ? C35 C36 H36A 109.2 . . ? C35 C36 H36B 109.2 8_565 . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? N1 C37 C6 173.1(11) . . ? C37 N1 C37 137.1(13) . 8 ? N2 C38 C7 167.9(12) . . ? C38 N2 C38 133.6(14) . 8 ? 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 C13 C1 C2 C3 4.4(11) . . . . ? C2 C1 C2 C3 -176.3(5) 8_565 . . . ? C13 C1 C2 C11 -175.2(6) . . . . ? C2 C1 C2 C11 4.2(12) 8_565 . . . ? C1 C2 C3 C4 -178.1(7) . . . . ? C11 C2 C3 C4 1.4(10) . . . . ? C2 C3 C4 C5 179.7(7) . . . . ? C2 C3 C4 C9 -2.3(11) . . . . ? C3 C4 C5 C6 -179.3(8) . . . . ? C9 C4 C5 C6 2.6(11) . . . . ? C4 C5 C6 C7 -2.6(12) . . . . ? C4 C5 C6 C37 -171.7(9) . . . . ? C5 C6 C7 C8 1.5(12) . . . . ? C37 C6 C7 C8 172.4(8) . . . . ? C5 C6 C7 C38 -170.7(8) . . . . ? C37 C6 C7 C38 0.1(12) . . . . ? C6 C7 C8 C9 -0.7(11) . . . . ? C38 C7 C8 C9 172.2(8) . . . . ? C7 C8 C9 C10 178.6(7) . . . . ? C7 C8 C9 C4 0.8(11) . . . . ? C3 C4 C9 C10 2.3(10) . . . . ? C5 C4 C9 C10 -179.5(6) . . . . ? C3 C4 C9 C8 -179.8(7) . . . . ? C5 C4 C9 C8 -1.7(10) . . . . ? C8 C9 C10 C11 -179.3(7) . . . . ? C4 C9 C10 C11 -1.6(10) . . . . ? C9 C10 C11 C12 -179.9(7) . . . . ? C9 C10 C11 C2 0.7(9) . . . . ? C3 C2 C11 C10 -0.5(9) . . . . ? C1 C2 C11 C10 179.0(6) . . . . ? C3 C2 C11 C12 180.0(6) . . . . ? C1 C2 C11 C12 -0.4(9) . . . . ? C10 C11 C12 C11 177.3(5) . . . 8_565 ? C2 C11 C12 C11 -3.3(12) . . . 8_565 ? C10 C11 C12 C25 -3.3(10) . . . . ? C2 C11 C12 C25 176.1(6) . . . . ? C14 Si1 C15 C16 -174.7(11) . . . . ? C15' Si1 C15 C16 65.1(12) 8_565 . . . ? C15' Si1 C15 C16 34(2) . . . . ? C21 Si1 C15 C16 -64.3(13) . . . . ? C15 Si1 C15 C16 81.0(16) 8_565 . . . ? C14 Si1 C15 C20 62.4(11) . . . . ? C15' Si1 C15 C20 -57.8(14) 8_565 . . . ? C15' Si1 C15 C20 -89(3) . . . . ? C21 Si1 C15 C20 172.8(10) . . . . ? C15 Si1 C15 C20 -41.9(19) 8_565 . . . ? C20 C15 C16 C17 -55.4(19) . . . . ? Si1 C15 C16 C17 -178.6(12) . . . . ? C15 C16 C17 C18 54(2) . . . . ? C16 C17 C18 C19 -55(2) . . . . ? C17 C18 C19 C20 58.8(18) . . . . ? C18 C19 C20 C15 -60.4(17) . . . . ? C16 C15 C20 C19 59.9(17) . . . . ? Si1 C15 C20 C19 -174.8(10) . . . . ? C14 Si1 C15' C16' -159.5(10) . . . . ? C15' Si1 C15' C16' 80.8(14) 8_565 . . . ? C21 Si1 C15' C16' -37.6(14) . . . . ? C15 Si1 C15' C16' 91.0(11) 8_565 . . . ? C15 Si1 C15' C16' -128(3) . . . . ? C14 Si1 C15' C20' -23.9(19) . . . . ? C15' Si1 C15' C20' -143.7(15) 8_565 . . . ? C21 Si1 C15' C20' 98.0(17) . . . . ? C15 Si1 C15' C20' -133.4(18) 8_565 . . . ? C15 Si1 C15' C20' 8(2) . . . . ? C20' C15' C16' C17' 45(2) . . . . ? Si1 C15' C16' C17' -179.8(11) . . . . ? C15' C16' C17' C18' -46(2) . . . . ? C16' C17' C18' C19' 52(3) . . . . ? C17' C18' C19' C20' -52(3) . . . . ? C16' C15' C20' C19' -48(3) . . . . ? Si1 C15' C20' C19' 176.7(15) . . . . ? C18' C19' C20' C15' 49(3) . . . . ? C14 Si1 C21 C22 -62.1(5) . . . 8_565 ? C15' Si1 C21 C22 64.3(8) 8_565 . . 8_565 ? C15' Si1 C21 C22 171.5(7) . . . 8_565 ? C15 Si1 C21 C22 42.4(8) 8_565 . . 8_565 ? C15 Si1 C21 C22 -166.7(7) . . . 8_565 ? C14 Si1 C21 C22 62.1(5) . . . . ? C15' Si1 C21 C22 -171.5(7) 8_565 . . . ? C15' Si1 C21 C22 -64.2(8) . . . . ? C15 Si1 C21 C22 166.7(7) 8_565 . . . ? C15 Si1 C21 C22 -42.4(8) . . . . ? C22 C21 C22 C23 -50.9(10) 8_565 . . . ? Si1 C21 C22 C23 -177.8(5) . . . . ? C21 C22 C23 C24 58.0(10) . . . . ? C22 C23 C24 C23 -60.3(13) . . . 8_565 ? C26 Si2 C27 C32 -169.8(5) . . . . ? C33 Si2 C27 C32 -55.7(6) . . . . ? C27 Si2 C27 C32 74.2(6) 8_565 . . . ? C26 Si2 C27 C28 60.5(5) . . . . ? C33 Si2 C27 C28 174.6(5) . . . . ? C27 Si2 C27 C28 -55.5(6) 8_565 . . . ? C32 C27 C28 C29 56.5(7) . . . . ? Si2 C27 C28 C29 -172.0(4) . . . . ? C27 C28 C29 C30 -55.8(7) . . . . ? C28 C29 C30 C31 56.1(8) . . . . ? C29 C30 C31 C32 -57.5(9) . . . . ? C28 C27 C32 C31 -55.7(8) . . . . ? Si2 C27 C32 C31 172.9(5) . . . . ? C30 C31 C32 C27 56.1(8) . . . . ? C26 Si2 C33 C34 -61.3(5) . . . 8_565 ? C27 Si2 C33 C34 -174.3(5) . . . 8_565 ? C27 Si2 C33 C34 51.6(6) 8_565 . . 8_565 ? C26 Si2 C33 C34 61.3(5) . . . . ? C27 Si2 C33 C34 -51.6(6) . . . . ? C27 Si2 C33 C34 174.3(5) 8_565 . . . ? C34 C33 C34 C35 -51.7(10) 8_565 . . . ? Si2 C33 C34 C35 -176.6(5) . . . . ? C33 C34 C35 C36 54.8(9) . . . . ? C34 C35 C36 C35 -55.7(12) . . . 8_565 ? C8 C7 C38 N2 153(5) . . . . ? C6 C7 C38 N2 -34(6) . . . . ? C7 C38 N2 C38 28(6) . . . 8 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.281 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.048 # Attachment 'x07119_DiCyanoTIBS.cif' data_x07119x _database_code_depnum_ccdc_archive 'CCDC 722606' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H64 N2 Si2' _chemical_formula_sum 'C50 H64 N2 Si2' _chemical_formula_weight 749.21 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' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? _symmetry_space_group_name_Hall ? 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 15.4450(10) _cell_length_b 8.7029(6) _cell_length_c 34.257(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.428(3) _cell_angle_gamma 90.00 _cell_volume 4566.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8185 _exptl_absorpt_correction_T_max 0.9721 _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 18 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 7782 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 69.54 _reflns_number_total 7782 _reflns_number_gt 7338 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker-AXS, 2006)' _computing_data_reduction 'APEX2 (Bruker-AXS, 2006)' _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^)+(0.0461P)^2^+72.5242P] 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 SHELXL _refine_ls_extinction_coef 0.00000(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7782 _refine_ls_number_parameters 659 _refine_ls_number_restraints 415 _refine_ls_R_factor_all 0.1842 _refine_ls_R_factor_gt 0.1793 _refine_ls_wR_factor_ref 0.3887 _refine_ls_wR_factor_gt 0.3862 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 1.415 _refine_ls_shift/su_mean 0.008 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 0.87706(14) 0.7044(3) 0.16368(6) 0.0229(5) Uani 1 1 d . . . Si2 Si 0.6446(2) 0.2488(4) -0.15428(8) 0.0588(11) Uani 1 1 d D . . C1 C 0.8057(5) 0.5402(9) 0.0403(2) 0.0218(16) Uani 1 1 d . A . C2 C 0.7232(5) 0.5800(10) 0.0215(2) 0.0247(17) Uani 1 1 d . . . C3 C 0.6665(5) 0.6742(10) 0.0387(2) 0.0270(18) Uani 1 1 d . . . H3 H 0.6845 0.7136 0.0644 0.032 Uiso 1 1 calc R . . C4 C 0.5850(5) 0.7128(10) 0.0201(2) 0.0268(18) Uani 1 1 d . . . C5 C 0.5273(5) 0.8115(11) 0.0385(2) 0.032(2) Uani 1 1 d . B . H5 H 0.5462 0.8534 0.0638 0.038 Uiso 1 1 calc R . . C6 C 0.4472(6) 0.8451(12) 0.0205(3) 0.038(2) Uani 1 1 d . . . C7 C 0.4190(5) 0.7824(11) -0.0178(3) 0.036(2) Uani 1 1 d . B . C8 C 0.4699(5) 0.6893(11) -0.0365(3) 0.033(2) Uani 1 1 d . . . H8 H 0.4494 0.6477 -0.0617 0.040 Uiso 1 1 calc R B . C9 C 0.5567(5) 0.6545(10) -0.0173(2) 0.0246(17) Uani 1 1 d . B . C10 C 0.6120(5) 0.5580(10) -0.0357(2) 0.0244(17) Uani 1 1 d . . . H10 H 0.5926 0.5172 -0.0610 0.029 Uiso 1 1 calc R B . C11 C 0.6941(5) 0.5219(10) -0.0172(2) 0.0224(16) Uani 1 1 d . B . C12 C 0.7506(5) 0.4249(9) -0.0359(2) 0.0182(15) Uani 1 1 d . . . C13 C 0.8329(5) 0.3863(10) -0.0165(2) 0.0215(16) Uani 1 1 d . B . C14 C 0.8898(5) 0.2876(10) -0.0347(2) 0.0229(16) Uani 1 1 d . . . H14 H 0.8716 0.2499 -0.0605 0.027 Uiso 1 1 calc R B . C15 C 0.9698(5) 0.2463(10) -0.0158(2) 0.0244(17) Uani 1 1 d . B . C16 C 1.0282(5) 0.1475(10) -0.0329(2) 0.0279(18) Uani 1 1 d . . . H16 H 1.0106 0.1061 -0.0584 0.034 Uiso 1 1 calc R B . C17 C 1.1070(5) 0.1115(10) -0.0142(3) 0.0308(19) Uani 1 1 d . B . C18 C 1.1366(5) 0.1733(10) 0.0246(2) 0.0288(19) Uani 1 1 d . . . C19 C 1.0838(5) 0.2656(10) 0.0421(2) 0.0265(17) Uani 1 1 d . B . H19 H 1.1031 0.3033 0.0678 0.032 Uiso 1 1 calc R . . C20 C 0.9991(5) 0.3093(10) 0.0232(2) 0.0222(16) Uani 1 1 d . . . C21 C 0.9443(4) 0.4000(9) 0.0405(2) 0.0188(15) Uani 1 1 d . B . H21 H 0.9628 0.4361 0.0664 0.023 Uiso 1 1 calc R . . C22 C 0.8618(5) 0.4434(9) 0.0222(2) 0.0187(15) Uani 1 1 d . . . C23 C 0.8339(5) 0.5943(11) 0.0793(2) 0.0293(19) Uani 1 1 d . . . C24 C 0.8529(6) 0.6404(11) 0.1122(2) 0.033(2) Uani 1 1 d . A . C25 C 0.9627(5) 0.5824(12) 0.1916(2) 0.034(2) Uani 1 1 d . A . H25A H 0.9602 0.6011 0.2200 0.040 Uiso 1 1 calc R . . H25B H 0.9455 0.4740 0.1864 0.040 Uiso 1 1 calc R . . C26 C 1.0571(5) 0.5968(12) 0.1850(2) 0.033(2) Uani 1 1 d . . . H26 H 1.0739 0.7074 0.1882 0.040 Uiso 1 1 calc R A . C27 C 1.0720(6) 0.5468(13) 0.1435(2) 0.041(2) Uani 1 1 d . A . H27A H 1.0489 0.4429 0.1384 0.061 Uiso 1 1 calc R . . H27B H 1.1347 0.5476 0.1414 0.061 Uiso 1 1 calc R . . H27C H 1.0419 0.6181 0.1242 0.061 Uiso 1 1 calc R . . C28 C 1.1164(6) 0.5046(12) 0.2155(2) 0.036(2) Uani 1 1 d . A . H28A H 1.1103 0.5427 0.2420 0.055 Uiso 1 1 calc R . . H28B H 1.1772 0.5159 0.2106 0.055 Uiso 1 1 calc R . . H28C H 1.0998 0.3959 0.2136 0.055 Uiso 1 1 calc R . . C29 C 0.9189(6) 0.9061(12) 0.1625(3) 0.039(2) Uani 1 1 d . A . H29A H 0.9237 0.9474 0.1896 0.047 Uiso 1 1 calc R . . H29B H 0.9788 0.9014 0.1552 0.047 Uiso 1 1 calc R . . C30 C 0.8680(7) 1.0206(13) 0.1356(3) 0.049(3) Uani 1 1 d . . . H30 H 0.8650 0.9721 0.1090 0.059 Uiso 1 1 calc R A . C31 C 0.9185(8) 1.1682(13) 0.1315(4) 0.060(3) Uani 1 1 d . A . H31A H 0.8989 1.2470 0.1488 0.090 Uiso 1 1 calc R . . H31B H 0.9082 1.2038 0.1041 0.090 Uiso 1 1 calc R . . H31C H 0.9810 1.1491 0.1389 0.090 Uiso 1 1 calc R . . C32 C 0.7790(10) 1.042(2) 0.1406(6) 0.114(7) Uani 1 1 d . A . H32A H 0.7472 0.9457 0.1354 0.172 Uiso 1 1 calc R . . H32B H 0.7534 1.1215 0.1223 0.172 Uiso 1 1 calc R . . H32C H 0.7752 1.0753 0.1677 0.172 Uiso 1 1 calc R . . C33 C 0.7770(7) 0.6845(13) 0.1885(3) 0.045(2) Uani 0.637(15) 1 d PDU A 1 H33A H 0.7908 0.7124 0.2166 0.054 Uiso 0.637(15) 1 calc PR A 1 H33B H 0.7314 0.7556 0.1763 0.054 Uiso 0.637(15) 1 calc PR A 1 C34 C 0.7418(10) 0.5138(19) 0.1849(5) 0.047(3) Uani 0.637(15) 1 d PDU A 1 H34 H 0.7920 0.4437 0.1823 0.056 Uiso 0.637(15) 1 calc PR A 1 C35 C 0.7033(12) 0.471(3) 0.2223(5) 0.067(4) Uani 0.637(15) 1 d PDU A 1 H35A H 0.7486 0.4800 0.2451 0.101 Uiso 0.637(15) 1 calc PR A 1 H35B H 0.6815 0.3655 0.2202 0.101 Uiso 0.637(15) 1 calc PR A 1 H35C H 0.6551 0.5412 0.2257 0.101 Uiso 0.637(15) 1 calc PR A 1 C36 C 0.6773(11) 0.498(2) 0.1492(5) 0.056(4) Uani 0.637(15) 1 d PDU A 1 H36A H 0.7046 0.5265 0.1260 0.084 Uiso 0.637(15) 1 calc PR A 1 H36B H 0.6273 0.5651 0.1514 0.084 Uiso 0.637(15) 1 calc PR A 1 H36C H 0.6574 0.3909 0.1467 0.084 Uiso 0.637(15) 1 calc PR A 1 C33' C 0.7770(7) 0.6845(13) 0.1885(3) 0.045(2) Uani 0.363(15) 1 d PDU A 2 H33C H 0.7829 0.7615 0.2100 0.054 Uiso 0.363(15) 1 calc PR A 2 H33D H 0.7279 0.7193 0.1691 0.054 Uiso 0.363(15) 1 calc PR A 2 C34' C 0.7451(14) 0.533(2) 0.2070(7) 0.048(3) Uiso 0.363(15) 1 d PDU A 2 H34' H 0.7960 0.4802 0.2225 0.058 Uiso 0.363(15) 1 calc PR A 2 C35' C 0.6781(19) 0.575(4) 0.2343(8) 0.063(7) Uiso 0.363(15) 1 d PDU A 2 H35D H 0.7057 0.6412 0.2555 0.094 Uiso 0.363(15) 1 calc PR A 2 H35E H 0.6564 0.4815 0.2456 0.094 Uiso 0.363(15) 1 calc PR A 2 H35F H 0.6293 0.6302 0.2193 0.094 Uiso 0.363(15) 1 calc PR A 2 C36' C 0.709(2) 0.432(3) 0.1740(8) 0.060(6) Uiso 0.363(15) 1 d PDU A 2 H36D H 0.7539 0.4110 0.1570 0.089 Uiso 0.363(15) 1 calc PR A 2 H36E H 0.6592 0.4836 0.1586 0.089 Uiso 0.363(15) 1 calc PR A 2 H36F H 0.6891 0.3352 0.1844 0.089 Uiso 0.363(15) 1 calc PR A 2 C37 C 0.7232(5) 0.3695(11) -0.0744(2) 0.0277(19) Uani 1 1 d . B . C38 C 0.6967(6) 0.3238(12) -0.1072(3) 0.038(2) Uani 1 1 d . B . C39 C 0.7234(6) 0.1388(12) -0.1800(3) 0.0378(18) Uani 0.518(6) 1 d PDU B 1 H39A H 0.6902 0.1020 -0.2049 0.045 Uiso 0.518(6) 1 calc PR B 1 H39B H 0.7661 0.2147 -0.1875 0.045 Uiso 0.518(6) 1 calc PR B 1 C40 C 0.7749(11) 0.0066(18) -0.1631(4) 0.037(3) Uani 0.518(6) 1 d PDU B 1 H40 H 0.7319 -0.0688 -0.1549 0.045 Uiso 0.518(6) 1 calc PR B 1 C41 C 0.8364(12) 0.040(3) -0.1276(5) 0.038(4) Uani 0.518(6) 1 d PDU B 1 H41A H 0.8663 -0.0546 -0.1181 0.057 Uiso 0.518(6) 1 calc PR B 1 H41B H 0.8044 0.0818 -0.1071 0.057 Uiso 0.518(6) 1 calc PR B 1 H41C H 0.8795 0.1156 -0.1340 0.057 Uiso 0.518(6) 1 calc PR B 1 C42 C 0.8209(13) -0.074(2) -0.1941(6) 0.045(5) Uani 0.518(6) 1 d PDU B 1 H42A H 0.8531 -0.1633 -0.1821 0.068 Uiso 0.518(6) 1 calc PR B 1 H42B H 0.8617 -0.0031 -0.2042 0.068 Uiso 0.518(6) 1 calc PR B 1 H42C H 0.7775 -0.1090 -0.2157 0.068 Uiso 0.518(6) 1 calc PR B 1 C39' C 0.7234(6) 0.1388(12) -0.1800(3) 0.0378(18) Uani 0.482(6) 1 d PDU B 2 H39C H 0.6961 0.1170 -0.2072 0.045 Uiso 0.482(6) 1 calc PR B 2 H39D H 0.7753 0.2039 -0.1818 0.045 Uiso 0.482(6) 1 calc PR B 2 C40' C 0.7523(12) -0.0076(18) -0.1609(5) 0.039(3) Uani 0.482(6) 1 d PDU B 2 H40' H 0.6980 -0.0582 -0.1541 0.046 Uiso 0.482(6) 1 calc PR B 2 C41' C 0.8104(15) 0.006(3) -0.1234(5) 0.045(5) Uani 0.482(6) 1 d PDU B 2 H41D H 0.8237 -0.0971 -0.1126 0.067 Uiso 0.482(6) 1 calc PR B 2 H41E H 0.7814 0.0661 -0.1047 0.067 Uiso 0.482(6) 1 calc PR B 2 H41F H 0.8647 0.0568 -0.1280 0.067 Uiso 0.482(6) 1 calc PR B 2 C42' C 0.7906(14) -0.119(2) -0.1884(7) 0.044(5) Uani 0.482(6) 1 d PDU B 2 H42D H 0.8073 -0.2145 -0.1742 0.066 Uiso 0.482(6) 1 calc PR B 2 H42E H 0.8423 -0.0726 -0.1975 0.066 Uiso 0.482(6) 1 calc PR B 2 H42F H 0.7470 -0.1412 -0.2111 0.066 Uiso 0.482(6) 1 calc PR B 2 C43 C 0.5615(10) 0.085(2) -0.1331(6) 0.043(3) Uani 0.518(6) 1 d PDU B 1 H43A H 0.5960 0.0318 -0.1108 0.051 Uiso 0.518(6) 1 calc PR B 1 H43B H 0.5150 0.1427 -0.1222 0.051 Uiso 0.518(6) 1 calc PR B 1 C44 C 0.5152(11) -0.043(2) -0.1608(6) 0.050(3) Uani 0.518(6) 1 d PDU B 1 H44 H 0.5623 -0.0882 -0.1747 0.060 Uiso 0.518(6) 1 calc PR B 1 C45 C 0.4869(13) -0.174(2) -0.1350(6) 0.056(4) Uani 0.518(6) 1 d PDU B 1 H45A H 0.5361 -0.2031 -0.1154 0.083 Uiso 0.518(6) 1 calc PR B 1 H45B H 0.4685 -0.2626 -0.1516 0.083 Uiso 0.518(6) 1 calc PR B 1 H45C H 0.4382 -0.1389 -0.1216 0.083 Uiso 0.518(6) 1 calc PR B 1 C46 C 0.4495(12) 0.016(3) -0.1923(6) 0.056(4) Uani 0.518(6) 1 d PDU B 1 H46A H 0.4756 0.0971 -0.2068 0.084 Uiso 0.518(6) 1 calc PR B 1 H46B H 0.3997 0.0579 -0.1807 0.084 Uiso 0.518(6) 1 calc PR B 1 H46C H 0.4294 -0.0679 -0.2103 0.084 Uiso 0.518(6) 1 calc PR B 1 C43' C 0.5541(11) 0.171(3) -0.1478(6) 0.042(4) Uani 0.482(6) 1 d PDU B 2 H43C H 0.5664 0.1053 -0.1242 0.051 Uiso 0.482(6) 1 calc PR B 2 H43D H 0.5159 0.2550 -0.1407 0.051 Uiso 0.482(6) 1 calc PR B 2 C44' C 0.4967(11) 0.071(2) -0.1797(6) 0.051(3) Uani 0.482(6) 1 d PDU B 2 H44' H 0.5369 -0.0096 -0.1879 0.061 Uiso 0.482(6) 1 calc PR B 2 C45' C 0.4278(12) -0.017(3) -0.1598(7) 0.059(4) Uani 0.482(6) 1 d PDU B 2 H45D H 0.4565 -0.0728 -0.1369 0.088 Uiso 0.482(6) 1 calc PR B 2 H45E H 0.3972 -0.0897 -0.1786 0.088 Uiso 0.482(6) 1 calc PR B 2 H45F H 0.3857 0.0562 -0.1513 0.088 Uiso 0.482(6) 1 calc PR B 2 C46' C 0.4656(12) 0.158(3) -0.2159(6) 0.053(4) Uani 0.482(6) 1 d PDU B 2 H46D H 0.5151 0.2087 -0.2256 0.079 Uiso 0.482(6) 1 calc PR B 2 H46E H 0.4229 0.2348 -0.2100 0.079 Uiso 0.482(6) 1 calc PR B 2 H46F H 0.4380 0.0867 -0.2360 0.079 Uiso 0.482(6) 1 calc PR B 2 C47 C 0.6379(12) 0.439(3) -0.1917(5) 0.050(3) Uani 0.518(6) 1 d PDU B 1 H47A H 0.6914 0.5018 -0.1860 0.060 Uiso 0.518(6) 1 calc PR B 1 H47B H 0.6327 0.4046 -0.2195 0.060 Uiso 0.518(6) 1 calc PR B 1 C48 C 0.5596(12) 0.530(2) -0.1849(4) 0.050(3) Uani 0.518(6) 1 d PDU B 1 H48 H 0.5082 0.4595 -0.1869 0.061 Uiso 0.518(6) 1 calc PR B 1 C49 C 0.5651(14) 0.609(3) -0.1481(5) 0.054(5) Uani 0.518(6) 1 d PDU B 1 H49A H 0.5101 0.6631 -0.1463 0.081 Uiso 0.518(6) 1 calc PR B 1 H49B H 0.6131 0.6835 -0.1462 0.081 Uiso 0.518(6) 1 calc PR B 1 H49C H 0.5758 0.5348 -0.1265 0.081 Uiso 0.518(6) 1 calc PR B 1 C50 C 0.5449(19) 0.648(3) -0.2204(6) 0.055(5) Uani 0.518(6) 1 d PDU B 1 H50A H 0.4924 0.7095 -0.2184 0.083 Uiso 0.518(6) 1 calc PR B 1 H50B H 0.5377 0.5920 -0.2454 0.083 Uiso 0.518(6) 1 calc PR B 1 H50C H 0.5955 0.7169 -0.2195 0.083 Uiso 0.518(6) 1 calc PR B 1 C47' C 0.5715(14) 0.390(3) -0.1830(6) 0.052(3) Uani 0.482(6) 1 d PDU B 2 H47C H 0.5304 0.3323 -0.2022 0.063 Uiso 0.482(6) 1 calc PR B 2 H47D H 0.5365 0.4417 -0.1646 0.063 Uiso 0.482(6) 1 calc PR B 2 C48' C 0.6135(13) 0.512(3) -0.2051(5) 0.054(3) Uani 0.482(6) 1 d PDU B 2 H48' H 0.6532 0.4577 -0.2214 0.064 Uiso 0.482(6) 1 calc PR B 2 C49' C 0.5572(19) 0.604(3) -0.2312(7) 0.064(6) Uani 0.482(6) 1 d PDU B 2 H49D H 0.5918 0.6770 -0.2445 0.096 Uiso 0.482(6) 1 calc PR B 2 H49E H 0.5172 0.6603 -0.2165 0.096 Uiso 0.482(6) 1 calc PR B 2 H49F H 0.5235 0.5381 -0.2509 0.096 Uiso 0.482(6) 1 calc PR B 2 C50' C 0.6740(14) 0.607(3) -0.1730(6) 0.051(4) Uani 0.482(6) 1 d PDU B 2 H50D H 0.7048 0.6866 -0.1860 0.076 Uiso 0.482(6) 1 calc PR B 2 H50E H 0.7167 0.5377 -0.1584 0.076 Uiso 0.482(6) 1 calc PR B 2 H50F H 0.6382 0.6548 -0.1548 0.076 Uiso 0.482(6) 1 calc PR B 2 C51 C 0.3944(11) 0.952(2) 0.0416(5) 0.043(4) Uani 0.518(6) 1 d PDU B 1 N1 N 0.3495(10) 1.037(2) 0.0567(5) 0.050(4) Uani 0.518(6) 1 d PDU B 1 C52 C 0.3348(11) 0.8277(18) -0.0324(5) 0.036(4) Uani 0.518(6) 1 d PDU B 1 N2 N 0.2645(10) 0.8601(19) -0.0463(5) 0.046(4) Uani 0.518(6) 1 d PDU B 1 C51' C 1.1674(10) 0.011(2) -0.0275(5) 0.026(3) Uani 0.482(6) 1 d PDU B 2 N1' N 1.2146(10) -0.071(2) -0.0408(5) 0.044(4) Uani 0.482(6) 1 d PDU B 2 C52' C 1.2237(9) 0.145(2) 0.0454(5) 0.025(3) Uani 0.482(6) 1 d PDU B 2 N2' N 1.2935(9) 0.1178(18) 0.0615(4) 0.033(3) Uani 0.482(6) 1 d PDU B 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 0.0238(11) 0.0191(12) 0.0261(10) -0.0011(8) 0.0042(8) 0.0015(9) Si2 0.0603(19) 0.064(2) 0.0453(15) -0.0274(14) -0.0212(13) 0.0397(17) C1 0.022(4) 0.019(4) 0.026(4) -0.005(3) 0.007(3) 0.003(3) C2 0.028(4) 0.025(5) 0.021(3) 0.004(3) 0.001(3) 0.004(3) C3 0.023(4) 0.031(5) 0.028(4) -0.001(3) 0.010(3) 0.007(4) C4 0.025(4) 0.028(5) 0.030(4) 0.007(3) 0.013(3) 0.007(4) C5 0.029(4) 0.031(5) 0.039(4) 0.007(4) 0.016(3) 0.020(4) C6 0.025(4) 0.037(6) 0.055(6) 0.019(4) 0.018(4) 0.000(4) C7 0.022(4) 0.030(6) 0.055(5) 0.018(4) 0.006(4) 0.004(4) C8 0.024(4) 0.027(5) 0.048(5) 0.009(4) 0.003(3) 0.015(4) C9 0.024(4) 0.017(4) 0.034(4) 0.006(3) 0.005(3) 0.007(3) C10 0.017(4) 0.029(5) 0.028(4) 0.004(3) 0.002(3) 0.001(3) C11 0.021(4) 0.025(5) 0.021(3) -0.002(3) 0.004(3) 0.004(3) C12 0.018(4) 0.012(4) 0.025(3) 0.000(3) 0.005(3) 0.001(3) C13 0.015(3) 0.028(5) 0.022(3) -0.003(3) 0.006(3) 0.007(3) C14 0.028(4) 0.020(4) 0.022(3) -0.002(3) 0.010(3) 0.000(3) C15 0.020(4) 0.026(5) 0.030(4) -0.002(3) 0.012(3) 0.004(3) C16 0.022(4) 0.025(5) 0.039(4) 0.000(3) 0.014(3) 0.008(3) C17 0.030(4) 0.016(5) 0.049(5) 0.004(4) 0.018(4) 0.005(4) C18 0.021(4) 0.021(5) 0.046(5) 0.011(4) 0.011(3) 0.004(3) C19 0.023(4) 0.021(5) 0.036(4) 0.007(3) 0.004(3) 0.003(3) C20 0.020(4) 0.021(4) 0.027(4) 0.000(3) 0.009(3) -0.008(3) C21 0.013(3) 0.024(4) 0.020(3) -0.001(3) 0.005(3) 0.004(3) C22 0.019(4) 0.014(4) 0.024(3) -0.001(3) 0.007(3) 0.000(3) C23 0.030(4) 0.031(5) 0.026(4) 0.001(3) 0.002(3) 0.004(4) C24 0.032(5) 0.032(5) 0.036(5) 0.005(4) 0.001(3) 0.010(4) C25 0.031(4) 0.040(6) 0.029(4) 0.007(4) 0.004(3) -0.005(4) C26 0.029(4) 0.038(6) 0.031(4) -0.002(4) 0.001(3) 0.000(4) C27 0.041(5) 0.049(7) 0.031(4) -0.001(4) 0.001(4) -0.001(5) C28 0.029(4) 0.041(6) 0.039(5) 0.004(4) 0.001(3) -0.001(4) C29 0.028(5) 0.037(6) 0.050(5) -0.003(4) -0.002(4) -0.001(4) C30 0.048(6) 0.029(6) 0.069(7) 0.013(5) 0.006(5) -0.003(5) C31 0.060(7) 0.033(7) 0.086(8) 0.018(6) 0.009(6) 0.007(5) C32 0.086(11) 0.090(14) 0.174(18) 0.058(13) 0.040(11) 0.048(11) C33 0.043(4) 0.049(4) 0.046(4) 0.005(3) 0.014(3) 0.006(3) C34 0.042(5) 0.049(5) 0.052(5) 0.010(5) 0.018(4) 0.004(4) C35 0.064(8) 0.074(9) 0.067(7) 0.028(7) 0.019(7) -0.006(8) C36 0.046(8) 0.059(9) 0.065(7) -0.004(7) 0.017(6) 0.005(7) C33' 0.043(4) 0.049(4) 0.046(4) 0.005(3) 0.014(3) 0.006(3) C37 0.027(4) 0.032(5) 0.024(4) 0.001(3) 0.004(3) 0.014(4) C38 0.041(5) 0.035(6) 0.038(5) -0.005(4) 0.005(4) 0.021(4) C39 0.035(4) 0.040(4) 0.039(4) -0.002(3) 0.011(3) 0.009(3) C40 0.031(6) 0.041(6) 0.042(5) -0.003(4) 0.012(5) 0.014(5) C41 0.027(9) 0.047(10) 0.043(7) -0.004(7) 0.012(6) 0.010(8) C42 0.034(10) 0.055(11) 0.051(8) -0.018(8) 0.018(8) 0.002(8) C39' 0.035(4) 0.040(4) 0.039(4) -0.002(3) 0.011(3) 0.009(3) C40' 0.033(6) 0.042(6) 0.043(5) -0.002(5) 0.011(5) 0.016(5) C41' 0.037(10) 0.051(11) 0.047(7) -0.003(7) 0.010(7) 0.020(9) C42' 0.029(9) 0.050(9) 0.053(8) -0.011(8) 0.005(8) 0.010(8) C43 0.017(6) 0.044(8) 0.068(8) -0.019(7) 0.006(6) 0.009(6) C44 0.030(6) 0.046(7) 0.074(8) -0.019(6) 0.005(5) 0.002(6) C45 0.042(10) 0.041(10) 0.083(12) -0.017(7) 0.007(9) 0.003(8) C46 0.036(8) 0.050(9) 0.077(9) -0.025(7) -0.009(7) 0.005(7) C43' 0.016(6) 0.038(8) 0.072(8) -0.018(7) 0.001(6) 0.005(6) C44' 0.025(6) 0.045(8) 0.080(8) -0.025(6) 0.001(6) 0.004(6) C45' 0.024(7) 0.053(10) 0.099(11) -0.026(8) 0.007(7) 0.006(7) C46' 0.030(8) 0.049(10) 0.077(9) -0.033(7) -0.006(7) 0.018(8) C47 0.048(7) 0.065(8) 0.039(6) 0.003(6) 0.010(5) -0.003(6) C48 0.048(6) 0.061(8) 0.043(6) 0.005(5) 0.009(5) -0.002(6) C49 0.062(11) 0.053(12) 0.046(7) 0.001(7) 0.007(8) 0.003(9) C50 0.051(9) 0.073(11) 0.041(8) 0.006(8) 0.002(8) -0.001(8) C47' 0.050(7) 0.063(8) 0.044(6) 0.003(6) 0.006(6) -0.004(6) C48' 0.052(7) 0.064(8) 0.046(6) 0.005(6) 0.010(5) -0.004(6) C49' 0.055(11) 0.086(14) 0.051(11) 0.015(9) 0.001(9) -0.006(11) C50' 0.055(10) 0.054(11) 0.044(9) 0.005(8) 0.010(7) -0.003(8) C51 0.030(9) 0.048(11) 0.051(9) 0.014(8) 0.000(7) 0.023(8) N1 0.038(8) 0.053(11) 0.058(9) 0.014(7) 0.005(7) 0.027(7) C52 0.045(8) 0.006(8) 0.054(9) 0.006(6) -0.007(7) 0.001(7) N2 0.043(8) 0.024(8) 0.068(10) 0.009(7) -0.003(7) 0.011(7) C51' 0.018(7) 0.027(9) 0.033(8) 0.002(6) 0.006(6) 0.007(6) N1' 0.033(8) 0.040(10) 0.055(9) -0.006(7) -0.002(7) 0.020(7) C52' 0.021(7) 0.021(8) 0.037(8) 0.000(6) 0.014(6) 0.004(6) N2' 0.026(7) 0.021(8) 0.052(8) 0.004(6) 0.007(6) 0.008(6) _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 C24 1.840(9) . ? Si1 C25 1.862(9) . ? Si1 C33 1.865(10) . ? Si1 C29 1.873(10) . ? Si2 C43' 1.595(19) . ? Si2 C38 1.828(9) . ? Si2 C39 1.857(9) . ? Si2 C47' 1.86(2) . ? Si2 C47 2.09(2) . ? Si2 C43 2.11(2) . ? C1 C2 1.396(10) . ? C1 C22 1.409(10) . ? C1 C23 1.432(10) . ? C2 C3 1.387(11) . ? C2 C11 1.436(10) . ? C3 C4 1.377(11) . ? C3 H3 0.9500 . ? C4 C9 1.394(11) . ? C4 C5 1.442(11) . ? C5 C6 1.341(12) . ? C5 H5 0.9500 . ? C6 C7 1.436(14) . ? C6 C51 1.483(18) . ? C7 C8 1.347(13) . ? C7 C52 1.389(17) . ? C8 C9 1.447(11) . ? C8 H8 0.9500 . ? C9 C10 1.403(11) . ? C10 C11 1.378(10) . ? C10 H10 0.9500 . ? C11 C12 1.424(10) . ? C12 C13 1.397(10) . ? C12 C37 1.415(10) . ? C13 C14 1.429(10) . ? C13 C22 1.431(10) . ? C14 C15 1.366(11) . ? C14 H14 0.9500 . ? C15 C16 1.426(10) . ? C15 C20 1.461(10) . ? C16 C17 1.337(12) . ? C16 H16 0.9500 . ? C17 C51' 1.396(16) . ? C17 C18 1.454(12) . ? C18 C19 1.340(12) . ? C18 C52' 1.459(16) . ? C19 C20 1.435(11) . ? C19 H19 0.9500 . ? C20 C21 1.349(11) . ? C21 C22 1.398(10) . ? C21 H21 0.9500 . ? C23 C24 1.197(12) . ? C25 C26 1.508(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C28 1.526(12) . ? C26 C27 1.533(11) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.508(14) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C32 1.420(17) . ? C30 C31 1.519(15) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.581(18) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C36 1.48(2) . ? C34 C35 1.53(2) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C34' C36' 1.48(2) . ? C34' C35' 1.53(2) . ? C34' H34' 1.0000 . ? C35' H35D 0.9800 . ? C35' H35E 0.9800 . ? C35' H35F 0.9800 . ? C36' H36D 0.9800 . ? C36' H36E 0.9800 . ? C36' H36F 0.9800 . ? C37 C38 1.212(12) . ? C39 C40 1.474(15) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.471(15) . ? C40 C42 1.524(15) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C40' C41' 1.472(16) . ? C40' C42' 1.523(16) . ? C40' H40' 1.0000 . ? C41' H41D 0.9800 . ? C41' H41E 0.9800 . ? C41' H41F 0.9800 . ? C42' H42D 0.9800 . ? C42' H42E 0.9800 . ? C42' H42F 0.9800 . ? C43 C44 1.574(18) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C46 1.48(2) . ? C44 C45 1.54(2) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C43' C44' 1.575(18) . ? C43' H43C 0.9900 . ? C43' H43D 0.9900 . ? C44' C46' 1.48(2) . ? C44' C45' 1.54(2) . ? C44' H44' 1.0000 . ? C45' H45D 0.9800 . ? C45' H45E 0.9800 . ? C45' H45F 0.9800 . ? C46' H46D 0.9800 . ? C46' H46E 0.9800 . ? C46' H46F 0.9800 . ? C47 C48 1.49(2) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.43(2) . ? C48 C50 1.59(2) . ? C48 H48 1.0000 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C47' C48' 1.50(2) . ? C47' H47C 0.9900 . ? C47' H47D 0.9900 . ? C48' C49' 1.41(2) . ? C48' C50' 1.58(2) . ? C48' H48' 1.0000 . ? C49' H49D 0.9800 . ? C49' H49E 0.9800 . ? C49' H49F 0.9800 . ? C50' H50D 0.9800 . ? C50' H50E 0.9800 . ? C50' H50F 0.9800 . ? C51 N1 1.180(16) . ? C52 N2 1.161(15) . ? C51' N1' 1.158(16) . ? C52' N2' 1.171(15) . ? 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 C24 Si1 C25 111.2(4) . . ? C24 Si1 C33 109.4(4) . . ? C25 Si1 C33 106.8(4) . . ? C24 Si1 C29 106.9(4) . . ? C25 Si1 C29 108.8(4) . . ? C33 Si1 C29 113.9(5) . . ? C43' Si2 C38 108.9(7) . . ? C43' Si2 C39 119.1(8) . . ? C38 Si2 C39 111.2(4) . . ? C43' Si2 C47' 82.6(10) . . ? C38 Si2 C47' 113.5(8) . . ? C39 Si2 C47' 118.6(7) . . ? C43' Si2 C47 116.5(10) . . ? C38 Si2 C47 103.9(7) . . ? C39 Si2 C47 95.8(6) . . ? C47' Si2 C47 34.2(9) . . ? C43' Si2 C43 23.3(8) . . ? C38 Si2 C43 99.0(6) . . ? C39 Si2 C43 106.2(6) . . ? C47' Si2 C43 105.9(8) . . ? C47 Si2 C43 139.7(8) . . ? C2 C1 C22 121.5(7) . . ? C2 C1 C23 119.9(7) . . ? C22 C1 C23 118.6(7) . . ? C3 C2 C1 122.6(7) . . ? C3 C2 C11 117.6(7) . . ? C1 C2 C11 119.8(7) . . ? C4 C3 C2 122.3(7) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C9 119.9(7) . . ? C3 C4 C5 121.5(8) . . ? C9 C4 C5 118.7(7) . . ? C6 C5 C4 121.0(9) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 119.4(9) . . ? C5 C6 C51 116.4(11) . . ? C7 C6 C51 124.2(10) . . ? C8 C7 C52 125.2(11) . . ? C8 C7 C6 122.4(8) . . ? C52 C7 C6 112.3(11) . . ? C7 C8 C9 118.2(8) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? C4 C9 C10 119.5(7) . . ? C4 C9 C8 120.3(7) . . ? C10 C9 C8 120.2(7) . . ? C11 C10 C9 120.6(7) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 120.7(7) . . ? C10 C11 C2 120.1(7) . . ? C12 C11 C2 119.2(7) . . ? C13 C12 C37 120.4(7) . . ? C13 C12 C11 120.0(6) . . ? C37 C12 C11 119.6(6) . . ? C12 C13 C14 120.6(7) . . ? C12 C13 C22 120.9(7) . . ? C14 C13 C22 118.4(6) . . ? C15 C14 C13 121.5(7) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 123.1(7) . . ? C14 C15 C20 119.2(7) . . ? C16 C15 C20 117.7(7) . . ? C17 C16 C15 122.0(8) . . ? C17 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C16 C17 C51' 126.6(10) . . ? C16 C17 C18 120.7(8) . . ? C51' C17 C18 112.7(9) . . ? C19 C18 C17 119.6(7) . . ? C19 C18 C52' 117.3(10) . . ? C17 C18 C52' 123.1(9) . . ? C18 C19 C20 122.0(8) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C21 C20 C19 122.9(7) . . ? C21 C20 C15 119.0(7) . . ? C19 C20 C15 118.0(7) . . ? C20 C21 C22 123.2(7) . . ? C20 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C21 C22 C1 122.7(7) . . ? C21 C22 C13 118.7(6) . . ? C1 C22 C13 118.6(7) . . ? C24 C23 C1 176.6(9) . . ? C23 C24 Si1 176.7(9) . . ? C26 C25 Si1 120.8(6) . . ? C26 C25 H25A 107.1 . . ? Si1 C25 H25A 107.1 . . ? C26 C25 H25B 107.1 . . ? Si1 C25 H25B 107.1 . . ? H25A C25 H25B 106.8 . . ? C25 C26 C28 111.1(7) . . ? C25 C26 C27 112.3(7) . . ? C28 C26 C27 109.7(8) . . ? C25 C26 H26 107.8 . . ? C28 C26 H26 107.9 . . ? C27 C26 H26 107.9 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 Si1 118.6(7) . . ? C30 C29 H29A 107.7 . . ? Si1 C29 H29A 107.7 . . ? C30 C29 H29B 107.7 . . ? Si1 C29 H29B 107.7 . . ? H29A C29 H29B 107.1 . . ? C32 C30 C29 116.8(10) . . ? C32 C30 C31 114.5(12) . . ? C29 C30 C31 112.4(9) . . ? C32 C30 H30 103.7 . . ? C29 C30 H30 103.7 . . ? C31 C30 H30 103.7 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.4 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 Si1 110.4(8) . . ? C34 C33 H33A 109.6 . . ? Si1 C33 H33A 109.6 . . ? C34 C33 H33B 109.6 . . ? Si1 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? C36 C34 C35 112.2(13) . . ? C36 C34 C33 110.0(13) . . ? C35 C34 C33 109.2(14) . . ? C36 C34 H34 108.5 . . ? C35 C34 H34 108.5 . . ? C33 C34 H34 108.5 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C36' C34' C35' 113.0(16) . . ? C36' C34' H34' 109.3 . . ? C35' C34' H34' 109.4 . . ? C34' C35' H35D 109.5 . . ? C34' C35' H35E 109.5 . . ? H35D C35' H35E 109.5 . . ? C34' C35' H35F 109.5 . . ? H35D C35' H35F 109.5 . . ? H35E C35' H35F 109.5 . . ? C34' C36' H36D 109.5 . . ? C34' C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? C34' C36' H36F 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? C38 C37 C12 177.7(8) . . ? C37 C38 Si2 173.1(9) . . ? C40 C39 Si2 124.6(8) . . ? C40 C39 H39A 106.2 . . ? Si2 C39 H39A 106.2 . . ? C40 C39 H39B 106.2 . . ? Si2 C39 H39B 106.2 . . ? H39A C39 H39B 106.4 . . ? C41 C40 C39 115.3(13) . . ? C41 C40 C42 110.9(12) . . ? C39 C40 C42 111.3(12) . . ? C41 C40 H40 106.2 . . ? C39 C40 H40 106.2 . . ? C42 C40 H40 106.2 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41' C40' C42' 110.3(12) . . ? C41' C40' H40' 105.6 . . ? C42' C40' H40' 105.6 . . ? C40' C41' H41D 109.5 . . ? C40' C41' H41E 109.5 . . ? H41D C41' H41E 109.5 . . ? C40' C41' H41F 109.5 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? C40' C42' H42D 109.5 . . ? C40' C42' H42E 109.5 . . ? H42D C42' H42E 109.5 . . ? C40' C42' H42F 109.5 . . ? H42D C42' H42F 109.5 . . ? H42E C42' H42F 109.5 . . ? C44 C43 Si2 121.5(13) . . ? C44 C43 H43A 107.0 . . ? Si2 C43 H43A 106.9 . . ? C44 C43 H43B 106.9 . . ? Si2 C43 H43B 107.0 . . ? H43A C43 H43B 106.7 . . ? C46 C44 C45 117.3(14) . . ? C46 C44 C43 114.2(16) . . ? C45 C44 C43 108.7(15) . . ? C46 C44 H44 105.2 . . ? C45 C44 H44 105.2 . . ? C43 C44 H44 105.2 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44' C43' Si2 124.3(14) . . ? C44' C43' H43C 106.2 . . ? Si2 C43' H43C 106.2 . . ? C44' C43' H43D 106.3 . . ? Si2 C43' H43D 106.2 . . ? H43C C43' H43D 106.4 . . ? C46' C44' C45' 117.0(14) . . ? C46' C44' C43' 113.1(17) . . ? C45' C44' C43' 109.2(15) . . ? C46' C44' H44' 105.5 . . ? C45' C44' H44' 105.5 . . ? C43' C44' H44' 105.5 . . ? C44' C45' H45D 109.5 . . ? C44' C45' H45E 109.5 . . ? H45D C45' H45E 109.5 . . ? C44' C45' H45F 109.5 . . ? H45D C45' H45F 109.5 . . ? H45E C45' H45F 109.5 . . ? C44' C46' H46D 109.5 . . ? C44' C46' H46E 109.5 . . ? H46D C46' H46E 109.5 . . ? C44' C46' H46F 109.5 . . ? H46D C46' H46F 109.5 . . ? H46E C46' H46F 109.5 . . ? C48 C47 Si2 107.7(11) . . ? C48 C47 H47A 110.2 . . ? Si2 C47 H47A 110.2 . . ? C48 C47 H47B 110.2 . . ? Si2 C47 H47B 110.2 . . ? H47A C47 H47B 108.5 . . ? C49 C48 C47 116.0(15) . . ? C49 C48 C50 110.6(16) . . ? C47 C48 C50 105.3(14) . . ? C49 C48 H48 108.2 . . ? C47 C48 H48 108.2 . . ? C50 C48 H48 108.2 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48' C47' Si2 117.5(13) . . ? C48' C47' H47C 107.9 . . ? Si2 C47' H47C 107.9 . . ? C48' C47' H47D 107.9 . . ? Si2 C47' H47D 107.9 . . ? H47C C47' H47D 107.2 . . ? C49' C48' C47' 116.7(16) . . ? C49' C48' C50' 113.9(18) . . ? C47' C48' C50' 106.0(13) . . ? C49' C48' H48' 106.5 . . ? C47' C48' H48' 106.5 . . ? C50' C48' H48' 106.5 . . ? C48' C49' H49D 109.5 . . ? C48' C49' H49E 109.5 . . ? H49D C49' H49E 109.5 . . ? C48' C49' H49F 109.5 . . ? H49D C49' H49F 109.5 . . ? H49E C49' H49F 109.5 . . ? C48' C50' H50D 109.5 . . ? C48' C50' H50E 109.5 . . ? H50D C50' H50E 109.5 . . ? C48' C50' H50F 109.5 . . ? H50D C50' H50F 109.5 . . ? H50E C50' H50F 109.5 . . ? N1 C51 C6 176.7(18) . . ? N2 C52 C7 176(2) . . ? N1' C51' C17 175.7(17) . . ? N2' C52' C18 177.6(18) . . ? 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 C22 C1 C2 C3 179.6(8) . . . . ? C23 C1 C2 C3 1.5(13) . . . . ? C22 C1 C2 C11 -0.1(12) . . . . ? C23 C1 C2 C11 -178.2(8) . . . . ? C1 C2 C3 C4 -179.8(8) . . . . ? C11 C2 C3 C4 -0.1(13) . . . . ? C2 C3 C4 C9 1.0(13) . . . . ? C2 C3 C4 C5 -179.7(8) . . . . ? C3 C4 C5 C6 -178.2(9) . . . . ? C9 C4 C5 C6 1.0(13) . . . . ? C4 C5 C6 C7 -0.4(14) . . . . ? C4 C5 C6 C51 -178.1(12) . . . . ? C5 C6 C7 C8 0.5(14) . . . . ? C51 C6 C7 C8 178.0(13) . . . . ? C5 C6 C7 C52 179.9(11) . . . . ? C51 C6 C7 C52 -2.5(17) . . . . ? C52 C7 C8 C9 179.4(11) . . . . ? C6 C7 C8 C9 -1.2(14) . . . . ? C3 C4 C9 C10 -0.6(13) . . . . ? C5 C4 C9 C10 -179.9(8) . . . . ? C3 C4 C9 C8 177.5(8) . . . . ? C5 C4 C9 C8 -1.8(12) . . . . ? C7 C8 C9 C4 1.8(13) . . . . ? C7 C8 C9 C10 179.9(8) . . . . ? C4 C9 C10 C11 -0.7(13) . . . . ? C8 C9 C10 C11 -178.8(8) . . . . ? C9 C10 C11 C12 -179.5(8) . . . . ? C9 C10 C11 C2 1.5(13) . . . . ? C3 C2 C11 C10 -1.1(12) . . . . ? C1 C2 C11 C10 178.6(8) . . . . ? C3 C2 C11 C12 179.9(8) . . . . ? C1 C2 C11 C12 -0.4(12) . . . . ? C10 C11 C12 C13 -178.4(8) . . . . ? C2 C11 C12 C13 0.5(12) . . . . ? C10 C11 C12 C37 2.2(12) . . . . ? C2 C11 C12 C37 -178.8(8) . . . . ? C37 C12 C13 C14 -1.4(12) . . . . ? C11 C12 C13 C14 179.2(8) . . . . ? C37 C12 C13 C22 179.1(8) . . . . ? C11 C12 C13 C22 -0.2(12) . . . . ? C12 C13 C14 C15 -178.8(8) . . . . ? C22 C13 C14 C15 0.7(12) . . . . ? C13 C14 C15 C16 179.7(8) . . . . ? C13 C14 C15 C20 -2.4(12) . . . . ? C14 C15 C16 C17 178.5(8) . . . . ? C20 C15 C16 C17 0.5(13) . . . . ? C15 C16 C17 C51' 176.9(12) . . . . ? C15 C16 C17 C18 -0.4(13) . . . . ? C16 C17 C18 C19 1.0(13) . . . . ? C51' C17 C18 C19 -176.7(10) . . . . ? C16 C17 C18 C52' -176.3(11) . . . . ? C51' C17 C18 C52' 6.1(16) . . . . ? C17 C18 C19 C20 -1.6(13) . . . . ? C52' C18 C19 C20 175.7(10) . . . . ? C18 C19 C20 C21 178.9(8) . . . . ? C18 C19 C20 C15 1.7(12) . . . . ? C14 C15 C20 C21 3.6(12) . . . . ? C16 C15 C20 C21 -178.4(8) . . . . ? C14 C15 C20 C19 -179.2(7) . . . . ? C16 C15 C20 C19 -1.1(11) . . . . ? C19 C20 C21 C22 179.8(7) . . . . ? C15 C20 C21 C22 -3.2(12) . . . . ? C20 C21 C22 C1 -179.0(8) . . . . ? C20 C21 C22 C13 1.4(12) . . . . ? C2 C1 C22 C21 -179.1(8) . . . . ? C23 C1 C22 C21 -1.1(12) . . . . ? C2 C1 C22 C13 0.5(12) . . . . ? C23 C1 C22 C13 178.5(8) . . . . ? C12 C13 C22 C21 179.3(7) . . . . ? C14 C13 C22 C21 -0.1(11) . . . . ? C12 C13 C22 C1 -0.3(12) . . . . ? C14 C13 C22 C1 -179.7(7) . . . . ? C2 C1 C23 C24 23(17) . . . . ? C22 C1 C23 C24 -155(17) . . . . ? C1 C23 C24 Si1 42(28) . . . . ? C25 Si1 C24 C23 94(14) . . . . ? C33 Si1 C24 C23 -24(15) . . . . ? C29 Si1 C24 C23 -148(14) . . . . ? C24 Si1 C25 C26 73.8(8) . . . . ? C33 Si1 C25 C26 -167.0(7) . . . . ? C29 Si1 C25 C26 -43.6(9) . . . . ? Si1 C25 C26 C28 171.0(7) . . . . ? Si1 C25 C26 C27 -65.7(11) . . . . ? C24 Si1 C29 C30 49.2(9) . . . . ? C25 Si1 C29 C30 169.3(8) . . . . ? C33 Si1 C29 C30 -71.7(9) . . . . ? Si1 C29 C30 C32 56.3(16) . . . . ? Si1 C29 C30 C31 -168.4(8) . . . . ? C24 Si1 C33 C34 55.6(10) . . . . ? C25 Si1 C33 C34 -64.9(9) . . . . ? C29 Si1 C33 C34 175.1(8) . . . . ? Si1 C33 C34 C36 -91.4(12) . . . . ? Si1 C33 C34 C35 145.1(11) . . . . ? C13 C12 C37 C38 168(26) . . . . ? C11 C12 C37 C38 -12(26) . . . . ? C12 C37 C38 Si2 -36(31) . . . . ? C43' Si2 C38 C37 -7(7) . . . . ? C39 Si2 C38 C37 -140(7) . . . . ? C47' Si2 C38 C37 83(7) . . . . ? C47 Si2 C38 C37 118(7) . . . . ? C43 Si2 C38 C37 -29(7) . . . . ? C43' Si2 C39 C40 -71.8(15) . . . . ? C38 Si2 C39 C40 56.1(13) . . . . ? C47' Si2 C39 C40 -169.6(13) . . . . ? C47 Si2 C39 C40 163.5(13) . . . . ? C43 Si2 C39 C40 -50.7(13) . . . . ? Si2 C39 C40 C41 -62.4(18) . . . . ? Si2 C39 C40 C42 170.1(11) . . . . ? C43' Si2 C43 C44 77(2) . . . . ? C38 Si2 C43 C44 -165.7(13) . . . . ? C39 Si2 C43 C44 -50.4(15) . . . . ? C47' Si2 C43 C44 76.6(16) . . . . ? C47 Si2 C43 C44 69.9(18) . . . . ? Si2 C43 C44 C46 -66.6(19) . . . . ? Si2 C43 C44 C45 160.4(13) . . . . ? C38 Si2 C43' C44' -170.1(16) . . . . ? C39 Si2 C43' C44' -41(2) . . . . ? C47' Si2 C43' C44' 77.6(19) . . . . ? C47 Si2 C43' C44' 73(2) . . . . ? C43 Si2 C43' C44' -102(3) . . . . ? Si2 C43' C44' C46' -62(2) . . . . ? Si2 C43' C44' C45' 165.9(17) . . . . ? C43' Si2 C47 C48 37.8(17) . . . . ? C38 Si2 C47 C48 -82.0(13) . . . . ? C39 Si2 C47 C48 164.4(13) . . . . ? C47' Si2 C47 C48 29.4(15) . . . . ? C43 Si2 C47 C48 40.8(19) . . . . ? Si2 C47 C48 C49 70(2) . . . . ? Si2 C47 C48 C50 -166.9(14) . . . . ? C43' Si2 C47' C48' -174.0(17) . . . . ? C38 Si2 C47' C48' 78.6(17) . . . . ? C39 Si2 C47' C48' -54.8(18) . . . . ? C47 Si2 C47' C48' -1.6(15) . . . . ? C43 Si2 C47' C48' -173.9(15) . . . . ? Si2 C47' C48' C49' 170.9(18) . . . . ? Si2 C47' C48' C50' -61(2) . . . . ? C5 C6 C51 N1 172(39) . . . . ? C7 C6 C51 N1 -6(40) . . . . ? C8 C7 C52 N2 7(31) . . . . ? C6 C7 C52 N2 -172(30) . . . . ? C16 C17 C51' N1' 19(27) . . . . ? C18 C17 C51' N1' -163(26) . . . . ? C19 C18 C52' N2' 146(41) . . . . ? C17 C18 C52' N2' -36(42) . . . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 69.54 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 0.673 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.123