#Supplementary Material (ESI) for Journal of Materials Chemistry #This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Sang Ook Kang' _publ_contact_author_email SANGOK@KOREA.AC.KR _publ_section_title ; Intermolecular Peripheral 2,5-Bipyridyl Interactions by Cyclization of 1,1'-Silanylene Unit of 2,3,4,5-Aryl Substituted Siloles: Enhanced Thermal Stability, High Charge Carrier Mobility, and Their Application to Electron Transporting Layers for OLEDs ; loop_ _publ_author_name 'Sang Ook Kang' 'Dae Won Cho' 'Won-Sik Han' 'Ah-Reum Hwang' 'Jaejung Ko' 'Soonnam Kwon' 'Su-Hyun Lee' ; H.-J.Son ; 'Il-Hwan Suh' 'Kyung Ryang Wee' # Attachment '3-Cy5.cif' data_3-Cy5 _database_code_depnum_ccdc_archive 'CCDC 742040' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H32 N4 Si' _chemical_formula_sum 'C40 H32 N4 Si' _chemical_formula_weight 596.79 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 monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.862(5) _cell_length_b 12.213(3) _cell_length_c 10.898(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.596(5) _cell_angle_gamma 90.00 _cell_volume 3155.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1963 _cell_measurement_theta_min 2.586 _cell_measurement_theta_max 20.974 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9563 _exptl_absorpt_correction_T_max 0.9762 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15594 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.27 _reflns_number_total 3915 _reflns_number_gt 2130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SMART (Bruker, 1999)' _computing_data_reduction 'SAINT-Plus (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+1.5756P] 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 0.0006(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3915 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1107 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1536 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si Si 0.5000 0.24371(7) 0.2500 0.0410(2) Uani 1 2 d S . . N1 N 0.25581(8) 0.04194(17) 0.07098(18) 0.0559(5) Uani 1 1 d . . . N2 N 0.37179(7) 0.22572(13) 0.14683(16) 0.0412(4) Uani 1 1 d . . . C1 C 0.44393(9) 0.35072(16) 0.2218(2) 0.0426(5) Uani 1 1 d . . . C2 C 0.46831(9) 0.45103(17) 0.2353(2) 0.0433(5) Uani 1 1 d . . . C3 C 0.43882(9) 0.55916(16) 0.2249(2) 0.0449(5) Uani 1 1 d . . . C4 C 0.43453(11) 0.6228(2) 0.3284(2) 0.0612(7) Uani 1 1 d . . . H4 H 0.4508 0.5987 0.4054 0.073 Uiso 1 1 calc R . . C5 C 0.40636(13) 0.7216(2) 0.3186(3) 0.0810(9) Uani 1 1 d . . . H5 H 0.4027 0.7625 0.3893 0.097 Uiso 1 1 calc R . . C6 C 0.38374(12) 0.7601(2) 0.2056(4) 0.0807(9) Uani 1 1 d . . . H6 H 0.3651 0.8271 0.1993 0.097 Uiso 1 1 calc R . . C7 C 0.38885(11) 0.6993(2) 0.1022(3) 0.0716(8) Uani 1 1 d . . . H7 H 0.3743 0.7257 0.0250 0.086 Uiso 1 1 calc R . . C8 C 0.41556(10) 0.59860(19) 0.1117(2) 0.0555(6) Uani 1 1 d . . . H8 H 0.4179 0.5570 0.0410 0.067 Uiso 1 1 calc R . . C9 C 0.38306(9) 0.32496(17) 0.20011(19) 0.0412(5) Uani 1 1 d . . . C10 C 0.33990(9) 0.39116(18) 0.2343(2) 0.0482(6) Uani 1 1 d . . . H10 H 0.3482 0.4589 0.2710 0.058 Uiso 1 1 calc R . . C11 C 0.28478(9) 0.35545(19) 0.2132(2) 0.0498(6) Uani 1 1 d . . . H11 H 0.2557 0.3990 0.2357 0.060 Uiso 1 1 calc R . . C12 C 0.27314(9) 0.25551(19) 0.1589(2) 0.0461(5) Uani 1 1 d . . . H12 H 0.2362 0.2302 0.1443 0.055 Uiso 1 1 calc R . . C13 C 0.31768(8) 0.19296(17) 0.12627(18) 0.0389(5) Uani 1 1 d . . . C14 C 0.30668(9) 0.08585(17) 0.06257(19) 0.0430(5) Uani 1 1 d . . . C15 C 0.34527(10) 0.03834(18) -0.0068(2) 0.0503(6) Uani 1 1 d . . . H15 H 0.3806 0.0696 -0.0094 0.060 Uiso 1 1 calc R . . C16 C 0.33041(11) -0.0563(2) -0.0721(2) 0.0599(7) Uani 1 1 d . . . H16 H 0.3554 -0.0888 -0.1206 0.072 Uiso 1 1 calc R . . C17 C 0.27858(12) -0.1016(2) -0.0646(2) 0.0627(7) Uani 1 1 d . . . H17 H 0.2676 -0.1654 -0.1074 0.075 Uiso 1 1 calc R . . C18 C 0.24331(12) -0.0504(2) 0.0076(2) 0.0645(7) Uani 1 1 d . . . H18 H 0.2082 -0.0820 0.0131 0.077 Uiso 1 1 calc R . . C19 C 0.51025(10) 0.14116(18) 0.1275(2) 0.0536(6) Uani 1 1 d . . . H19A H 0.4793 0.1436 0.0616 0.064 Uiso 1 1 calc R . . H19B H 0.5453 0.1542 0.0929 0.064 Uiso 1 1 calc R . . C20 C 0.5118(2) 0.0330(2) 0.1942(3) 0.1178(15) Uani 1 1 d . . . H20A H 0.4920 -0.0208 0.1398 0.141 Uiso 1 1 calc R . . H20B H 0.5508 0.0095 0.2104 0.141 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si 0.0408(5) 0.0310(4) 0.0505(5) 0.000 0.0017(4) 0.000 N1 0.0539(12) 0.0621(13) 0.0521(12) -0.0023(10) 0.0087(9) -0.0174(10) N2 0.0411(10) 0.0371(10) 0.0446(10) 0.0021(8) 0.0008(8) 0.0006(7) C1 0.0437(12) 0.0344(11) 0.0483(13) -0.0017(9) -0.0007(10) 0.0010(9) C2 0.0465(12) 0.0352(11) 0.0471(13) -0.0008(9) 0.0003(10) 0.0032(9) C3 0.0441(12) 0.0318(11) 0.0574(14) -0.0002(10) -0.0003(10) -0.0016(9) C4 0.0746(17) 0.0474(14) 0.0606(16) -0.0064(12) 0.0031(13) 0.0073(12) C5 0.093(2) 0.0484(16) 0.101(2) -0.0246(16) 0.0079(19) 0.0139(15) C6 0.0729(19) 0.0380(14) 0.127(3) -0.0021(17) -0.0058(19) 0.0145(13) C7 0.0697(18) 0.0465(15) 0.093(2) 0.0151(15) -0.0139(15) 0.0059(13) C8 0.0588(15) 0.0460(13) 0.0595(16) 0.0016(11) -0.0026(12) 0.0049(11) C9 0.0455(12) 0.0337(11) 0.0433(12) 0.0026(9) 0.0000(9) 0.0021(9) C10 0.0522(13) 0.0410(12) 0.0510(14) -0.0035(10) 0.0042(11) 0.0055(10) C11 0.0451(13) 0.0548(14) 0.0496(14) -0.0011(11) 0.0052(10) 0.0117(11) C12 0.0356(11) 0.0565(14) 0.0454(12) 0.0027(11) 0.0017(9) 0.0020(10) C13 0.0396(12) 0.0415(12) 0.0349(11) 0.0047(9) 0.0005(9) -0.0024(9) C14 0.0459(12) 0.0410(12) 0.0404(12) 0.0067(10) -0.0021(10) -0.0051(10) C15 0.0471(13) 0.0432(13) 0.0598(15) -0.0003(11) 0.0027(11) 0.0004(10) C16 0.0653(16) 0.0457(14) 0.0680(17) -0.0088(12) 0.0047(13) 0.0040(12) C17 0.0807(19) 0.0462(14) 0.0588(16) -0.0051(12) -0.0018(14) -0.0111(13) C18 0.0679(17) 0.0668(17) 0.0575(16) -0.0037(14) 0.0016(13) -0.0298(14) C19 0.0505(14) 0.0499(14) 0.0606(15) -0.0086(12) 0.0066(11) 0.0025(11) C20 0.209(5) 0.0396(16) 0.115(3) -0.0094(17) 0.062(3) 0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si C19 1.867(2) . ? Si C19 1.867(2) 2_655 ? Si C1 1.870(2) 2_655 ? Si C1 1.870(2) . ? N1 C18 1.339(3) . ? N1 C14 1.340(3) . ? N2 C13 1.346(3) . ? N2 C9 1.357(3) . ? C1 C2 1.357(3) . ? C1 C9 1.478(3) . ? C2 C3 1.494(3) . ? C2 C2 1.510(4) 2_655 ? C3 C8 1.380(3) . ? C3 C4 1.384(3) . ? C4 C5 1.380(3) . ? C4 H4 0.9300 . ? C5 C6 1.369(4) . ? C5 H5 0.9300 . ? C6 C7 1.367(4) . ? C6 H6 0.9300 . ? C7 C8 1.383(3) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.393(3) . ? C10 C11 1.380(3) . ? C10 H10 0.9300 . ? C11 C12 1.371(3) . ? C11 H11 0.9300 . ? C12 C13 1.388(3) . ? C12 H12 0.9300 . ? C13 C14 1.490(3) . ? C14 C15 1.384(3) . ? C15 C16 1.382(3) . ? C15 H15 0.9300 . ? C16 C17 1.366(4) . ? C16 H16 0.9300 . ? C17 C18 1.368(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.507(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C20 1.397(6) 2_655 ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? 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 C19 Si C19 95.73(16) . 2_655 ? C19 Si C1 115.85(10) . 2_655 ? C19 Si C1 120.10(10) 2_655 2_655 ? C19 Si C1 120.10(10) . . ? C19 Si C1 115.85(10) 2_655 . ? C1 Si C1 91.34(13) 2_655 . ? C18 N1 C14 116.9(2) . . ? C13 N2 C9 118.43(18) . . ? C2 C1 C9 127.63(19) . . ? C2 C1 Si 108.87(15) . . ? C9 C1 Si 123.28(15) . . ? C1 C2 C3 126.68(19) . . ? C1 C2 C2 115.44(12) . 2_655 ? C3 C2 C2 117.88(11) . 2_655 ? C8 C3 C4 118.2(2) . . ? C8 C3 C2 120.9(2) . . ? C4 C3 C2 120.8(2) . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C7 C6 C5 119.4(2) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C8 120.4(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C3 C8 C7 120.8(2) . . ? C3 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? N2 C9 C10 121.07(19) . . ? N2 C9 C1 113.67(18) . . ? C10 C9 C1 125.20(19) . . ? C11 C10 C9 119.5(2) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 119.7(2) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 118.5(2) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? N2 C13 C12 122.8(2) . . ? N2 C13 C14 116.93(18) . . ? C12 C13 C14 120.23(19) . . ? N1 C14 C15 122.3(2) . . ? N1 C14 C13 115.6(2) . . ? C15 C14 C13 122.00(19) . . ? C16 C15 C14 119.0(2) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C17 C16 C15 119.3(2) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 118.1(2) . . ? C16 C17 H17 121.0 . . ? C18 C17 H17 121.0 . . ? N1 C18 C17 124.5(2) . . ? N1 C18 H18 117.7 . . ? C17 C18 H18 117.7 . . ? C20 C19 Si 103.95(18) . . ? C20 C19 H19A 111.0 . . ? Si C19 H19A 111.0 . . ? C20 C19 H19B 111.0 . . ? Si C19 H19B 111.0 . . ? H19A C19 H19B 109.0 . . ? C20 C20 C19 115.5(2) 2_655 . ? C20 C20 H20A 108.4 2_655 . ? C19 C20 H20A 108.4 . . ? C20 C20 H20B 108.4 2_655 . ? C19 C20 H20B 108.4 . . ? H20A C20 H20B 107.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C19 Si C1 C2 -121.76(17) . . . . ? C19 Si C1 C2 124.09(17) 2_655 . . . ? C1 Si C1 C2 -0.58(12) 2_655 . . . ? C19 Si C1 C9 63.2(2) . . . . ? C19 Si C1 C9 -50.9(2) 2_655 . . . ? C1 Si C1 C9 -175.6(2) 2_655 . . . ? C9 C1 C2 C3 -3.2(4) . . . . ? Si C1 C2 C3 -177.94(19) . . . . ? C9 C1 C2 C2 176.3(2) . . . 2_655 ? Si C1 C2 C2 1.5(3) . . . 2_655 ? C1 C2 C3 C8 -72.1(3) . . . . ? C2 C2 C3 C8 108.4(3) 2_655 . . . ? C1 C2 C3 C4 108.4(3) . . . . ? C2 C2 C3 C4 -71.0(3) 2_655 . . . ? C8 C3 C4 C5 1.7(4) . . . . ? C2 C3 C4 C5 -178.8(2) . . . . ? C3 C4 C5 C6 -2.1(4) . . . . ? C4 C5 C6 C7 0.5(5) . . . . ? C5 C6 C7 C8 1.4(4) . . . . ? C4 C3 C8 C7 0.2(4) . . . . ? C2 C3 C8 C7 -179.3(2) . . . . ? C6 C7 C8 C3 -1.8(4) . . . . ? C13 N2 C9 C10 0.8(3) . . . . ? C13 N2 C9 C1 178.13(18) . . . . ? C2 C1 C9 N2 157.2(2) . . . . ? Si C1 C9 N2 -28.8(3) . . . . ? C2 C1 C9 C10 -25.5(4) . . . . ? Si C1 C9 C10 148.46(19) . . . . ? N2 C9 C10 C11 -0.2(3) . . . . ? C1 C9 C10 C11 -177.3(2) . . . . ? C9 C10 C11 C12 -0.1(3) . . . . ? C10 C11 C12 C13 -0.2(3) . . . . ? C9 N2 C13 C12 -1.0(3) . . . . ? C9 N2 C13 C14 177.35(17) . . . . ? C11 C12 C13 N2 0.7(3) . . . . ? C11 C12 C13 C14 -177.58(19) . . . . ? C18 N1 C14 C15 -0.7(3) . . . . ? C18 N1 C14 C13 175.5(2) . . . . ? N2 C13 C14 N1 163.63(18) . . . . ? C12 C13 C14 N1 -18.0(3) . . . . ? N2 C13 C14 C15 -20.1(3) . . . . ? C12 C13 C14 C15 158.3(2) . . . . ? N1 C14 C15 C16 1.6(3) . . . . ? C13 C14 C15 C16 -174.5(2) . . . . ? C14 C15 C16 C17 -1.3(4) . . . . ? C15 C16 C17 C18 0.2(4) . . . . ? C14 N1 C18 C17 -0.4(4) . . . . ? C16 C17 C18 N1 0.6(4) . . . . ? C19 Si C19 C20 -6.4(2) 2_655 . . . ? C1 Si C19 C20 121.1(2) 2_655 . . . ? C1 Si C19 C20 -130.8(2) . . . . ? Si C19 C20 C20 19.7(6) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.397 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.044 # Attachment '3-cy6.cif' data_k070605 _database_code_depnum_ccdc_archive 'CCDC 742041' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H34 N4 Si' _chemical_formula_sum 'C41 H34 N4 Si' _chemical_formula_weight 610.81 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 monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.1053(18) _cell_length_b 12.0672(9) _cell_length_c 11.2330(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.0750(10) _cell_angle_gamma 90.00 _cell_volume 3226.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4130 _cell_measurement_theta_min 2.541 _cell_measurement_theta_max 27.135 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.109 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9652 _exptl_absorpt_correction_T_max 0.9727 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16323 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.33 _reflns_number_total 4002 _reflns_number_gt 2663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SMART (Bruker, 1999)' _computing_data_reduction 'SAINT-Plus (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1148P)^2^+3.2935P] 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 4002 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.2090 _refine_ls_wR_factor_gt 0.1695 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si Si 0.5000 0.24433(6) 0.2500 0.0455(3) Uani 1 2 d S . . N1 N 0.25366(10) 0.0433(2) 0.0704(2) 0.0671(6) Uani 1 1 d . . . N2 N 0.37047(7) 0.22812(14) 0.14374(17) 0.0462(4) Uani 1 1 d . . . C1 C 0.44388(9) 0.35225(17) 0.2195(2) 0.0473(5) Uani 1 1 d . . . C2 C 0.46841(9) 0.45358(17) 0.2355(2) 0.0474(5) Uani 1 1 d . . . C3 C 0.43884(9) 0.56213(17) 0.2281(2) 0.0522(5) Uani 1 1 d . . . C4 C 0.43447(13) 0.6209(2) 0.3316(3) 0.0725(8) Uani 1 1 d . . . H4 H 0.4512 0.5935 0.4060 0.087 Uiso 1 1 calc R . . C5 C 0.40543(15) 0.7198(3) 0.3257(4) 0.0935(11) Uani 1 1 d . . . H5 H 0.4020 0.7577 0.3962 0.112 Uiso 1 1 calc R . . C6 C 0.38167(14) 0.7623(2) 0.2165(4) 0.0942(12) Uani 1 1 d . . . H6 H 0.3619 0.8288 0.2127 0.113 Uiso 1 1 calc R . . C7 C 0.38711(13) 0.7066(2) 0.1133(4) 0.0847(10) Uani 1 1 d . . . H7 H 0.3719 0.7364 0.0390 0.102 Uiso 1 1 calc R . . C8 C 0.41513(11) 0.6061(2) 0.1182(3) 0.0661(7) Uani 1 1 d . . . H8 H 0.4180 0.5682 0.0473 0.079 Uiso 1 1 calc R . . C9 C 0.38356(9) 0.32639(17) 0.1987(2) 0.0465(5) Uani 1 1 d . . . C10 C 0.34210(10) 0.39178(19) 0.2380(2) 0.0557(6) Uani 1 1 d . . . H10 H 0.3515 0.4590 0.2765 0.067 Uiso 1 1 calc R . . C11 C 0.28743(10) 0.3561(2) 0.2192(2) 0.0587(6) Uani 1 1 d . . . H11 H 0.2595 0.3992 0.2446 0.070 Uiso 1 1 calc R . . C12 C 0.27393(10) 0.2560(2) 0.1627(2) 0.0526(5) Uani 1 1 d . . . H12 H 0.2371 0.2304 0.1496 0.063 Uiso 1 1 calc R . . C13 C 0.31673(9) 0.19478(18) 0.12601(18) 0.0461(5) Uani 1 1 d . . . C14 C 0.30378(9) 0.08808(18) 0.0616(2) 0.0489(5) Uani 1 1 d . . . C15 C 0.33998(10) 0.04054(19) -0.0075(2) 0.0575(6) Uani 1 1 d . . . H15 H 0.3749 0.0723 -0.0108 0.069 Uiso 1 1 calc R . . C16 C 0.32369(12) -0.0547(2) -0.0717(3) 0.0689(7) Uani 1 1 d . . . H16 H 0.3472 -0.0877 -0.1196 0.083 Uiso 1 1 calc R . . C17 C 0.27220(13) -0.0998(2) -0.0637(3) 0.0721(8) Uani 1 1 d . . . H17 H 0.2599 -0.1635 -0.1064 0.086 Uiso 1 1 calc R . . C18 C 0.23990(14) -0.0493(3) 0.0080(3) 0.0758(8) Uani 1 1 d . . . H18 H 0.2054 -0.0816 0.0142 0.091 Uiso 1 1 calc R . . C19 C 0.51282(13) 0.1521(2) 0.1251(3) 0.0768(9) Uani 1 1 d . . . H19A H 0.4799 0.1533 0.0630 0.092 Uiso 1 1 calc R . . H19B H 0.5441 0.1814 0.0902 0.092 Uiso 1 1 calc R . . C20 C 0.5250(4) 0.0388(4) 0.1603(6) 0.177(3) Uani 1 1 d . . . H20A H 0.5169 -0.0051 0.0873 0.213 Uiso 1 1 calc R . . H20B H 0.5653 0.0347 0.1859 0.213 Uiso 1 1 calc R . . C21 C 0.5000 -0.0186(4) 0.2500 0.132(3) Uani 1 2 d S . . H21A H 0.5288 -0.0666 0.2926 0.158 Uiso 0.50 1 calc PR . . H21B H 0.4712 -0.0666 0.2074 0.158 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si 0.0470(5) 0.0326(4) 0.0578(5) 0.000 0.0113(4) 0.000 N1 0.0658(13) 0.0767(15) 0.0595(12) -0.0049(11) 0.0123(10) -0.0266(11) N2 0.0429(9) 0.0413(9) 0.0531(10) 0.0033(7) 0.0038(8) -0.0007(7) C1 0.0481(11) 0.0356(10) 0.0565(12) -0.0012(9) 0.0034(9) -0.0001(8) C2 0.0494(12) 0.0355(10) 0.0554(12) 0.0009(9) 0.0019(9) 0.0017(8) C3 0.0472(12) 0.0342(10) 0.0725(15) -0.0002(10) 0.0012(10) 0.0000(9) C4 0.0807(19) 0.0497(13) 0.0849(19) -0.0111(13) 0.0058(15) 0.0065(13) C5 0.091(2) 0.0556(16) 0.134(3) -0.0277(19) 0.017(2) 0.0114(16) C6 0.0695(19) 0.0392(13) 0.170(4) -0.0071(18) 0.006(2) 0.0115(12) C7 0.0665(17) 0.0530(15) 0.126(3) 0.0235(18) -0.0104(17) 0.0085(13) C8 0.0627(15) 0.0496(13) 0.0812(18) 0.0080(12) -0.0034(13) 0.0047(11) C9 0.0469(11) 0.0400(10) 0.0513(12) 0.0023(9) 0.0041(9) 0.0013(8) C10 0.0571(13) 0.0472(12) 0.0623(14) -0.0057(10) 0.0084(11) 0.0029(10) C11 0.0520(13) 0.0654(15) 0.0602(14) -0.0010(12) 0.0130(11) 0.0098(11) C12 0.0434(11) 0.0626(14) 0.0513(12) 0.0045(10) 0.0054(9) -0.0011(10) C13 0.0448(11) 0.0485(11) 0.0436(11) 0.0069(9) 0.0025(8) -0.0021(9) C14 0.0501(12) 0.0473(11) 0.0466(11) 0.0074(9) -0.0003(9) -0.0073(9) C15 0.0494(12) 0.0475(12) 0.0739(16) -0.0013(11) 0.0043(11) -0.0003(10) C16 0.0685(17) 0.0522(14) 0.0843(19) -0.0082(13) 0.0071(14) 0.0028(12) C17 0.087(2) 0.0550(15) 0.0699(17) -0.0053(13) -0.0008(15) -0.0171(14) C18 0.0800(19) 0.0787(19) 0.0672(16) -0.0066(14) 0.0071(14) -0.0395(16) C19 0.0692(17) 0.0713(18) 0.095(2) -0.0329(16) 0.0303(15) -0.0144(14) C20 0.308(9) 0.082(3) 0.150(5) -0.032(3) 0.061(5) 0.073(4) C21 0.091(4) 0.044(2) 0.266(10) 0.000 0.043(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 Si C19 1.854(3) . ? Si C19 1.854(3) 2_655 ? Si C1 1.870(2) 2_655 ? Si C1 1.870(2) . ? N1 C18 1.333(4) . ? N1 C14 1.341(3) . ? N2 C13 1.341(3) . ? N2 C9 1.351(3) . ? C1 C2 1.358(3) . ? C1 C9 1.469(3) . ? C2 C3 1.487(3) . ? C2 C2 1.506(4) 2_655 ? C3 C4 1.380(4) . ? C3 C8 1.382(4) . ? C4 C5 1.380(4) . ? C4 H4 0.9300 . ? C5 C6 1.369(6) . ? C5 H5 0.9300 . ? C6 C7 1.364(5) . ? C6 H6 0.9300 . ? C7 C8 1.385(4) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.398(3) . ? C10 C11 1.371(3) . ? C10 H10 0.9300 . ? C11 C12 1.379(3) . ? C11 H11 0.9300 . ? C12 C13 1.383(3) . ? C12 H12 0.9300 . ? C13 C14 1.486(3) . ? C14 C15 1.381(3) . ? C15 C16 1.381(4) . ? C15 H15 0.9300 . ? C16 C17 1.371(4) . ? C16 H16 0.9300 . ? C17 C18 1.350(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.441(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.431(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C20 1.431(7) 2_655 ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? 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 C19 Si C19 106.2(2) . 2_655 ? C19 Si C1 110.76(11) . 2_655 ? C19 Si C1 118.79(13) 2_655 2_655 ? C19 Si C1 118.79(13) . . ? C19 Si C1 110.76(11) 2_655 . ? C1 Si C1 91.73(13) 2_655 . ? C18 N1 C14 116.8(2) . . ? C13 N2 C9 118.80(19) . . ? C2 C1 C9 127.71(19) . . ? C2 C1 Si 108.39(15) . . ? C9 C1 Si 123.39(15) . . ? C1 C2 C3 126.2(2) . . ? C1 C2 C2 115.66(13) . 2_655 ? C3 C2 C2 118.12(12) . 2_655 ? C4 C3 C8 118.7(2) . . ? C4 C3 C2 120.3(2) . . ? C8 C3 C2 121.0(2) . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 120.3(3) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C7 C6 C5 119.6(3) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 120.6(3) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C3 C8 C7 120.1(3) . . ? C3 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? N2 C9 C10 120.8(2) . . ? N2 C9 C1 114.39(18) . . ? C10 C9 C1 124.7(2) . . ? C11 C10 C9 119.5(2) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 119.8(2) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 118.2(2) . . ? C11 C12 H12 120.9 . . ? C13 C12 H12 120.9 . . ? N2 C13 C12 122.9(2) . . ? N2 C13 C14 117.2(2) . . ? C12 C13 C14 119.9(2) . . ? N1 C14 C15 122.0(2) . . ? N1 C14 C13 115.8(2) . . ? C15 C14 C13 122.1(2) . . ? C16 C15 C14 119.1(2) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 118.8(3) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C18 C17 C16 118.2(3) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? N1 C18 C17 125.0(3) . . ? N1 C18 H18 117.5 . . ? C17 C18 H18 117.5 . . ? C20 C19 Si 114.4(3) . . ? C20 C19 H19A 108.7 . . ? Si C19 H19A 108.7 . . ? C20 C19 H19B 108.7 . . ? Si C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C21 C20 C19 124.2(5) . . ? C21 C20 H20A 106.3 . . ? C19 C20 H20A 106.3 . . ? C21 C20 H20B 106.3 . . ? C19 C20 H20B 106.3 . . ? H20A C20 H20B 106.4 . . ? C20 C21 C20 122.2(5) . 2_655 ? C20 C21 H21A 106.8 . . ? C20 C21 H21A 106.8 2_655 . ? C20 C21 H21B 106.8 . . ? C20 C21 H21B 106.8 2_655 . ? H21A C21 H21B 106.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.504 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.050 # start Validation Reply Form _vrf_PLAT241_k070605 ; PROBLEM: Check High Ueq as Compared to Neighbors for C20 RESPONSE: ...maybe because C20 is a terminal atom. ; # end Validation Reply Form # end Validation Reply Form # Attachment 'pypyspypy.cif' data_pypyspypy _database_code_depnum_ccdc_archive 'CCDC 742042' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H30 N4 Si' _chemical_formula_sum 'C38 H30 N4 Si' _chemical_formula_weight 570.75 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 monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.863(4) _cell_length_b 10.3528(18) _cell_length_c 26.024(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.721(4) _cell_angle_gamma 90.00 _cell_volume 6159.5(18) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6124 _cell_measurement_theta_min 2.293 _cell_measurement_theta_max 20.926 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9626 _exptl_absorpt_correction_T_max 0.9731 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61832 _diffrn_reflns_av_R_equivalents 0.0906 _diffrn_reflns_av_sigmaI/netI 0.1175 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.42 _reflns_number_total 15379 _reflns_number_gt 6066 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SMART (Bruker, 1999)' _computing_data_reduction 'SAINT-Plus (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+3.4345P] 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 0.0006(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 15379 _refine_ls_number_parameters 780 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1863 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.2004 _refine_ls_wR_factor_gt 0.1318 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 0.37222(4) 0.06691(9) -0.09311(4) 0.0519(3) Uani 1 1 d . . . Si2 Si 0.12804(4) 0.75788(9) 0.04902(3) 0.0500(2) Uani 1 1 d . . . N1 N 0.31850(10) -0.0369(2) -0.19784(9) 0.0476(6) Uani 1 1 d . . . N2 N 0.19255(11) -0.1102(2) -0.27586(9) 0.0498(6) Uani 1 1 d . . . N3 N 0.40053(11) 0.2016(2) 0.00723(10) 0.0514(7) Uani 1 1 d . . . N4 N 0.34628(15) 0.3295(3) 0.12543(13) 0.0843(10) Uani 1 1 d . . . N5 N 0.18589(13) 0.6741(3) -0.05027(9) 0.0545(7) Uani 1 1 d . . . N6 N 0.32070(18) 0.5899(4) -0.11014(14) 0.1066(14) Uani 1 1 d . . . N7 N 0.08588(10) 0.8646(2) 0.15690(9) 0.0477(6) Uani 1 1 d . . . N8 N 0.11635(16) 1.0174(3) 0.27666(13) 0.0909(11) Uani 1 1 d . . . C2 C 0.40699(13) 0.0008(3) -0.15176(12) 0.0516(8) Uani 1 1 d . . . C3 C 0.46447(13) 0.0330(3) -0.15146(12) 0.0494(8) Uani 1 1 d . . . C4 C 0.48530(13) 0.1024(3) -0.10388(12) 0.0474(8) Uani 1 1 d . . . C5 C 0.44508(13) 0.1182(3) -0.06693(12) 0.0492(8) Uani 1 1 d . . . C6 C 0.37531(13) -0.0729(3) -0.19149(12) 0.0504(8) Uani 1 1 d . . . C7 C 0.39794(14) -0.1753(4) -0.21872(13) 0.0629(9) Uani 1 1 d . . . H7 H 0.4367 -0.1997 -0.2136 0.075 Uiso 1 1 calc R . . C8 C 0.36357(15) -0.2408(4) -0.25319(15) 0.0702(10) Uani 1 1 d . . . H8 H 0.3784 -0.3106 -0.2714 0.084 Uiso 1 1 calc R . . C9 C 0.30696(14) -0.2019(4) -0.26040(13) 0.0617(9) Uani 1 1 d . . . H9 H 0.2830 -0.2442 -0.2841 0.074 Uiso 1 1 calc R . . C10 C 0.28549(13) -0.0999(3) -0.23240(11) 0.0467(8) Uani 1 1 d . . . C11 C 0.22396(13) -0.0571(3) -0.23764(11) 0.0450(7) Uani 1 1 d . . . C12 C 0.20011(15) 0.0285(3) -0.20381(13) 0.0629(10) Uani 1 1 d . . . H12 H 0.2232 0.0658 -0.1782 0.076 Uiso 1 1 calc R . . C13 C 0.14175(15) 0.0590(4) -0.20793(14) 0.0710(11) Uani 1 1 d . . . H13 H 0.1248 0.1163 -0.1850 0.085 Uiso 1 1 calc R . . C14 C 0.10911(15) 0.0037(3) -0.24626(13) 0.0612(9) Uani 1 1 d . . . H14 H 0.0694 0.0214 -0.2498 0.073 Uiso 1 1 calc R . . C15 C 0.13645(14) -0.0784(3) -0.27920(12) 0.0548(8) Uani 1 1 d . . . H15 H 0.1143 -0.1143 -0.3058 0.066 Uiso 1 1 calc R . . C16 C 0.50465(13) 0.0048(3) -0.19464(12) 0.0503(8) Uani 1 1 d . . . C17 C 0.49306(15) 0.0532(3) -0.24304(13) 0.0610(9) Uani 1 1 d . . . H17 H 0.4622 0.1105 -0.2479 0.073 Uiso 1 1 calc R . . C18 C 0.52633(19) 0.0182(4) -0.28407(15) 0.0818(12) Uani 1 1 d . . . H18 H 0.5176 0.0504 -0.3166 0.098 Uiso 1 1 calc R . . C19 C 0.5726(2) -0.0644(5) -0.27711(17) 0.0899(13) Uani 1 1 d . . . H19 H 0.5953 -0.0880 -0.3050 0.108 Uiso 1 1 calc R . . C20 C 0.58537(17) -0.1116(4) -0.22993(16) 0.0777(11) Uani 1 1 d . . . H20 H 0.6167 -0.1679 -0.2254 0.093 Uiso 1 1 calc R . . C21 C 0.55202(15) -0.0765(4) -0.18866(14) 0.0634(9) Uani 1 1 d . . . H21 H 0.5616 -0.1080 -0.1562 0.076 Uiso 1 1 calc R . . C22 C 0.54558(13) 0.1582(3) -0.10414(12) 0.0499(8) Uani 1 1 d . . . C23 C 0.59455(15) 0.0922(4) -0.08813(15) 0.0741(11) Uani 1 1 d . . . H23 H 0.5906 0.0084 -0.0757 0.089 Uiso 1 1 calc R . . C24 C 0.64901(17) 0.1466(6) -0.08998(17) 0.0927(14) Uani 1 1 d . . . H24 H 0.6817 0.0993 -0.0796 0.111 Uiso 1 1 calc R . . C25 C 0.6553(2) 0.2698(7) -0.10710(19) 0.1072(18) Uani 1 1 d . . . H25 H 0.6922 0.3076 -0.1079 0.129 Uiso 1 1 calc R . . C26 C 0.6077(2) 0.3376(5) -0.12303(19) 0.1079(17) Uani 1 1 d . . . H26 H 0.6120 0.4218 -0.1348 0.129 Uiso 1 1 calc R . . C27 C 0.55274(17) 0.2820(4) -0.12184(14) 0.0719(11) Uani 1 1 d . . . H27 H 0.5204 0.3290 -0.1331 0.086 Uiso 1 1 calc R . . C28 C 0.45183(14) 0.1764(3) -0.01621(12) 0.0511(8) Uani 1 1 d . . . C29 C 0.50476(15) 0.1999(4) 0.00926(13) 0.0667(10) Uani 1 1 d . . . H29 H 0.5399 0.1799 -0.0065 0.080 Uiso 1 1 calc R . . C30 C 0.50496(17) 0.2524(4) 0.05751(14) 0.0745(11) Uani 1 1 d . . . H30 H 0.5401 0.2673 0.0749 0.089 Uiso 1 1 calc R . . C31 C 0.45257(17) 0.2829(3) 0.08008(14) 0.0663(10) Uani 1 1 d . . . H31 H 0.4519 0.3223 0.1122 0.080 Uiso 1 1 calc R . . C32 C 0.40108(15) 0.2541(3) 0.05418(12) 0.0539(8) Uani 1 1 d . . . C33 C 0.34369(16) 0.2752(3) 0.07936(14) 0.0592(9) Uani 1 1 d . . . C34 C 0.2950(2) 0.3504(5) 0.14891(18) 0.1006(15) Uani 1 1 d . . . H34 H 0.2960 0.3880 0.1814 0.121 Uiso 1 1 calc R . . C35 C 0.2423(2) 0.3201(5) 0.12837(19) 0.0928(14) Uani 1 1 d . . . H35 H 0.2081 0.3379 0.1461 0.111 Uiso 1 1 calc R . . C36 C 0.24000(19) 0.2631(5) 0.08137(19) 0.0975(14) Uani 1 1 d . . . H36 H 0.2044 0.2389 0.0666 0.117 Uiso 1 1 calc R . . C37 C 0.29183(17) 0.2419(4) 0.05598(16) 0.0792(12) Uani 1 1 d . . . H37 H 0.2915 0.2054 0.0233 0.095 Uiso 1 1 calc R . . C38 C 0.32743(15) 0.2111(4) -0.10936(15) 0.0696(10) Uani 1 1 d . . . H38A H 0.3489 0.2663 -0.1320 0.104 Uiso 1 1 calc R . . H38B H 0.3184 0.2573 -0.0785 0.104 Uiso 1 1 calc R . . H38C H 0.2918 0.1843 -0.1260 0.104 Uiso 1 1 calc R . . C39 C 0.33057(16) -0.0540(4) -0.05644(14) 0.0737(11) Uani 1 1 d . . . H39A H 0.2989 -0.0863 -0.0773 0.111 Uiso 1 1 calc R . . H39B H 0.3152 -0.0145 -0.0261 0.111 Uiso 1 1 calc R . . H39C H 0.3559 -0.1241 -0.0468 0.111 Uiso 1 1 calc R . . C40 C 0.04416(13) 0.7955(3) 0.13239(11) 0.0452(7) Uani 1 1 d . . . C41 C 0.08148(14) 0.8845(3) 0.20723(12) 0.0512(8) Uani 1 1 d . . . C42 C 0.03693(15) 0.8319(4) 0.23634(13) 0.0633(10) Uani 1 1 d . . . H42 H 0.0349 0.8478 0.2714 0.076 Uiso 1 1 calc R . . C43 C -0.00392(14) 0.7561(4) 0.21192(13) 0.0628(10) Uani 1 1 d . . . H43 H -0.0334 0.7166 0.2306 0.075 Uiso 1 1 calc R . . C44 C -0.00114(13) 0.7389(3) 0.15977(12) 0.0538(8) Uani 1 1 d . . . H44 H -0.0293 0.6896 0.1427 0.065 Uiso 1 1 calc R . . C45 C 0.12898(18) 0.9620(3) 0.23198(14) 0.0649(10) Uani 1 1 d . . . C46 C 0.18338(19) 0.9721(4) 0.21007(17) 0.0843(12) Uani 1 1 d . . . H46 H 0.1909 0.9320 0.1789 0.101 Uiso 1 1 calc R . . C47 C 0.2265(2) 1.0420(5) 0.2348(2) 0.1170(18) Uani 1 1 d . . . H47 H 0.2634 1.0510 0.2206 0.140 Uiso 1 1 calc R . . C48 C 0.2135(3) 1.0982(5) 0.2810(3) 0.128(2) Uani 1 1 d . . . H48 H 0.2417 1.1452 0.2991 0.154 Uiso 1 1 calc R . . C49 C 0.1592(3) 1.0843(5) 0.2998(2) 0.124(2) Uani 1 1 d . . . H49 H 0.1510 1.1238 0.3310 0.148 Uiso 1 1 calc R . . C51 C -0.05178(13) 0.7702(3) 0.04619(12) 0.0501(8) Uani 1 1 d . . . C52 C -0.07837(15) 0.8809(4) 0.06454(13) 0.0610(9) Uani 1 1 d . . . H52 H -0.0556 0.9524 0.0731 0.073 Uiso 1 1 calc R . . C53 C -0.13784(17) 0.8863(5) 0.07025(15) 0.0782(12) Uani 1 1 d . . . H53 H -0.1552 0.9616 0.0823 0.094 Uiso 1 1 calc R . . C54 C -0.17150(18) 0.7823(6) 0.05839(16) 0.0902(14) Uani 1 1 d . . . H54 H -0.2118 0.7863 0.0626 0.108 Uiso 1 1 calc R . . C55 C -0.14640(18) 0.6714(5) 0.04023(16) 0.0829(13) Uani 1 1 d . . . H55 H -0.1696 0.6003 0.0322 0.099 Uiso 1 1 calc R . . C56 C -0.08646(15) 0.6653(4) 0.03380(13) 0.0623(9) Uani 1 1 d . . . H56 H -0.0695 0.5903 0.0211 0.075 Uiso 1 1 calc R . . C57 C -0.00489(14) 0.7312(3) -0.05826(11) 0.0494(8) Uani 1 1 d . . . C58 C -0.04022(14) 0.8345(3) -0.07197(12) 0.0546(8) Uani 1 1 d . . . H58 H -0.0404 0.9086 -0.0518 0.065 Uiso 1 1 calc R . . C59 C -0.07515(15) 0.8280(4) -0.11542(13) 0.0624(9) Uani 1 1 d . . . H59 H -0.0984 0.8982 -0.1246 0.075 Uiso 1 1 calc R . . C60 C -0.07588(15) 0.7190(4) -0.14510(13) 0.0639(10) Uani 1 1 d . . . H60 H -0.0993 0.7152 -0.1745 0.077 Uiso 1 1 calc R . . C61 C -0.04203(16) 0.6157(4) -0.13138(13) 0.0661(10) Uani 1 1 d . . . H61 H -0.0430 0.5410 -0.1512 0.079 Uiso 1 1 calc R . . C62 C -0.00670(15) 0.6216(3) -0.08853(13) 0.0619(9) Uani 1 1 d . . . H62 H 0.0164 0.5509 -0.0797 0.074 Uiso 1 1 calc R . . C63 C 0.13232(15) 0.7195(3) -0.06179(12) 0.0525(8) Uani 1 1 d . . . C64 C 0.11675(18) 0.7534(4) -0.11161(13) 0.0685(10) Uani 1 1 d . . . H64 H 0.0797 0.7859 -0.1190 0.082 Uiso 1 1 calc R . . C65 C 0.1567(2) 0.7383(4) -0.14990(15) 0.0859(14) Uani 1 1 d . . . H65 H 0.1469 0.7604 -0.1836 0.103 Uiso 1 1 calc R . . C66 C 0.2114(2) 0.6904(4) -0.13844(14) 0.0805(13) Uani 1 1 d . . . H66 H 0.2390 0.6793 -0.1640 0.097 Uiso 1 1 calc R . . C67 C 0.22428(16) 0.6593(3) -0.08808(13) 0.0591(9) Uani 1 1 d . . . C68 C 0.28309(18) 0.6083(3) -0.07264(15) 0.0675(11) Uani 1 1 d . . . C69 C 0.3736(3) 0.5435(6) -0.0956(3) 0.130(3) Uani 1 1 d . . . H69 H 0.4006 0.5287 -0.1214 0.156 Uiso 1 1 calc R . . C70 C 0.3906(2) 0.5168(5) -0.0473(3) 0.1077(18) Uani 1 1 d . . . H70 H 0.4279 0.4851 -0.0401 0.129 Uiso 1 1 calc R . . C71 C 0.3520(2) 0.5376(4) -0.0096(2) 0.1011(15) Uani 1 1 d . . . H71 H 0.3621 0.5211 0.0245 0.121 Uiso 1 1 calc R . . C72 C 0.29728(19) 0.5838(4) -0.02269(18) 0.0890(14) Uani 1 1 d . . . H72 H 0.2699 0.5983 0.0028 0.107 Uiso 1 1 calc R . . C73 C 0.17627(15) 0.9008(4) 0.04918(14) 0.0740(11) Uani 1 1 d . . . H73A H 0.2096 0.8841 0.0281 0.111 Uiso 1 1 calc R . . H73B H 0.1891 0.9188 0.0837 0.111 Uiso 1 1 calc R . . H73C H 0.1552 0.9738 0.0358 0.111 Uiso 1 1 calc R . . C74 C 0.16421(15) 0.6165(4) 0.07895(13) 0.0718(11) Uani 1 1 d . . . H74A H 0.1385 0.5433 0.0771 0.108 Uiso 1 1 calc R . . H74B H 0.1733 0.6353 0.1143 0.108 Uiso 1 1 calc R . . H74C H 0.1996 0.5975 0.0610 0.108 Uiso 1 1 calc R . . C102 C 0.05363(13) 0.7795(3) 0.07712(12) 0.0475(8) Uani 1 1 d . . . C103 C 0.01270(13) 0.7643(3) 0.03929(11) 0.0463(7) Uani 1 1 d . . . C104 C 0.03605(14) 0.7406(3) -0.01349(12) 0.0487(8) Uani 1 1 d . . . C105 C 0.09536(14) 0.7323(3) -0.01630(11) 0.0497(8) Uani 1 1 d . . . 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 0.0377(5) 0.0642(6) 0.0537(6) -0.0057(4) -0.0017(4) -0.0075(4) Si2 0.0435(5) 0.0668(6) 0.0397(5) 0.0008(4) -0.0037(4) 0.0003(4) N1 0.0398(14) 0.0579(16) 0.0450(15) -0.0041(12) -0.0004(12) -0.0058(12) N2 0.0457(16) 0.0613(17) 0.0423(15) -0.0058(12) -0.0058(12) -0.0063(13) N3 0.0503(16) 0.0532(16) 0.0505(16) -0.0015(13) -0.0007(13) -0.0031(13) N4 0.092(3) 0.085(2) 0.076(2) -0.0271(19) 0.017(2) -0.006(2) N5 0.0671(19) 0.0553(17) 0.0415(15) -0.0017(12) 0.0112(14) -0.0099(14) N6 0.077(3) 0.150(4) 0.094(3) -0.056(3) 0.044(2) -0.041(3) N7 0.0471(15) 0.0524(16) 0.0433(15) -0.0022(12) -0.0103(12) 0.0046(12) N8 0.116(3) 0.082(2) 0.074(2) -0.0328(19) -0.037(2) 0.024(2) C2 0.0404(18) 0.060(2) 0.054(2) -0.0030(16) -0.0076(15) -0.0056(15) C3 0.0422(18) 0.056(2) 0.0496(19) 0.0001(15) -0.0025(15) -0.0020(15) C4 0.0391(17) 0.054(2) 0.0492(19) 0.0015(15) -0.0087(15) -0.0043(14) C5 0.0424(17) 0.058(2) 0.0471(19) -0.0007(15) -0.0012(15) -0.0049(15) C6 0.0425(18) 0.060(2) 0.0488(19) -0.0053(16) 0.0006(15) -0.0040(15) C7 0.0421(19) 0.073(2) 0.073(2) -0.017(2) -0.0047(17) 0.0000(17) C8 0.055(2) 0.074(3) 0.082(3) -0.028(2) 0.0011(19) 0.0023(19) C9 0.049(2) 0.073(2) 0.063(2) -0.0171(19) -0.0043(17) -0.0069(18) C10 0.0417(17) 0.057(2) 0.0411(17) -0.0051(15) -0.0019(14) -0.0069(15) C11 0.0432(17) 0.0522(19) 0.0394(17) -0.0032(14) -0.0046(14) -0.0055(15) C12 0.052(2) 0.076(2) 0.061(2) -0.0219(19) -0.0172(17) 0.0038(18) C13 0.062(2) 0.080(3) 0.071(2) -0.027(2) -0.0168(19) 0.023(2) C14 0.050(2) 0.070(2) 0.063(2) -0.0089(19) -0.0161(17) 0.0083(18) C15 0.051(2) 0.064(2) 0.0498(19) -0.0017(17) -0.0141(16) -0.0027(17) C16 0.0409(18) 0.060(2) 0.0493(19) -0.0023(16) -0.0031(15) -0.0053(15) C17 0.062(2) 0.071(2) 0.049(2) 0.0023(18) -0.0040(18) 0.0029(18) C18 0.103(3) 0.094(3) 0.049(2) 0.003(2) 0.005(2) 0.009(3) C19 0.104(4) 0.101(3) 0.065(3) 0.000(2) 0.029(3) 0.018(3) C20 0.071(3) 0.084(3) 0.079(3) -0.002(2) 0.012(2) 0.015(2) C21 0.051(2) 0.080(3) 0.059(2) 0.0097(19) -0.0002(17) 0.0044(19) C22 0.0423(18) 0.063(2) 0.0445(18) -0.0005(16) -0.0043(14) -0.0099(16) C23 0.046(2) 0.086(3) 0.091(3) 0.009(2) -0.014(2) -0.0019(19) C24 0.042(2) 0.150(5) 0.085(3) -0.008(3) -0.012(2) -0.009(3) C25 0.058(3) 0.170(6) 0.094(4) -0.005(4) 0.000(3) -0.054(3) C26 0.093(4) 0.122(4) 0.109(4) 0.020(3) -0.008(3) -0.060(3) C27 0.068(3) 0.072(3) 0.075(3) 0.012(2) -0.007(2) -0.016(2) C28 0.0495(19) 0.057(2) 0.0465(19) 0.0010(15) -0.0027(15) -0.0088(16) C29 0.050(2) 0.095(3) 0.055(2) -0.005(2) -0.0059(17) -0.0176(19) C30 0.063(2) 0.106(3) 0.055(2) -0.011(2) -0.0106(19) -0.026(2) C31 0.075(3) 0.071(2) 0.052(2) -0.0085(18) -0.0048(19) -0.020(2) C32 0.063(2) 0.050(2) 0.0486(19) 0.0008(16) 0.0001(17) -0.0078(16) C33 0.070(2) 0.053(2) 0.055(2) 0.0019(17) 0.0061(18) -0.0037(18) C34 0.100(4) 0.115(4) 0.088(3) -0.037(3) 0.031(3) 0.001(3) C35 0.084(3) 0.102(4) 0.093(4) -0.006(3) 0.026(3) 0.014(3) C36 0.068(3) 0.133(4) 0.092(3) -0.009(3) 0.011(3) 0.004(3) C37 0.064(3) 0.105(3) 0.068(3) -0.014(2) 0.005(2) 0.001(2) C38 0.050(2) 0.081(3) 0.077(3) -0.009(2) -0.0062(18) -0.0027(19) C39 0.065(2) 0.083(3) 0.074(3) -0.007(2) 0.010(2) -0.020(2) C40 0.0382(17) 0.0502(18) 0.0470(18) -0.0001(15) -0.0088(14) 0.0092(14) C41 0.055(2) 0.054(2) 0.0442(19) -0.0028(15) -0.0127(16) 0.0148(16) C42 0.057(2) 0.088(3) 0.0444(19) -0.0030(19) 0.0022(17) 0.023(2) C43 0.0420(19) 0.090(3) 0.056(2) 0.0069(19) 0.0029(16) 0.0100(19) C44 0.0366(17) 0.071(2) 0.053(2) 0.0016(17) -0.0078(15) 0.0031(16) C45 0.083(3) 0.053(2) 0.058(2) -0.0056(18) -0.027(2) 0.0123(19) C46 0.074(3) 0.095(3) 0.083(3) -0.008(2) -0.024(2) -0.014(2) C47 0.103(4) 0.109(4) 0.138(5) -0.014(4) -0.050(4) -0.027(3) C48 0.153(6) 0.083(4) 0.147(6) -0.023(4) -0.086(5) -0.009(4) C49 0.165(6) 0.094(4) 0.110(4) -0.042(3) -0.074(5) 0.027(4) C51 0.0414(17) 0.063(2) 0.0454(18) 0.0029(16) -0.0099(14) -0.0018(16) C52 0.049(2) 0.069(2) 0.066(2) -0.0047(19) -0.0056(17) 0.0024(18) C53 0.057(2) 0.108(3) 0.070(3) -0.004(2) -0.001(2) 0.019(2) C54 0.044(2) 0.150(5) 0.077(3) 0.008(3) 0.002(2) -0.010(3) C55 0.068(3) 0.107(4) 0.073(3) 0.020(3) -0.017(2) -0.036(3) C56 0.059(2) 0.065(2) 0.062(2) 0.0085(18) -0.0186(18) -0.0082(18) C57 0.0553(19) 0.0494(19) 0.0431(17) 0.0010(15) -0.0142(15) -0.0028(15) C58 0.059(2) 0.052(2) 0.053(2) 0.0027(16) -0.0103(16) 0.0010(16) C59 0.061(2) 0.069(2) 0.057(2) 0.0104(19) -0.0104(18) 0.0084(18) C60 0.068(2) 0.080(3) 0.0439(19) 0.0000(19) -0.0201(17) -0.004(2) C61 0.077(3) 0.067(2) 0.054(2) -0.0104(18) -0.0204(19) -0.005(2) C62 0.071(2) 0.052(2) 0.062(2) -0.0026(17) -0.0234(18) 0.0047(18) C63 0.064(2) 0.050(2) 0.0432(19) -0.0012(15) -0.0021(16) -0.0067(17) C64 0.088(3) 0.073(3) 0.045(2) 0.0084(18) -0.006(2) -0.016(2) C65 0.127(4) 0.090(3) 0.041(2) 0.006(2) -0.003(3) -0.035(3) C66 0.116(4) 0.080(3) 0.046(2) -0.007(2) 0.024(2) -0.034(3) C67 0.076(3) 0.053(2) 0.048(2) -0.0068(16) 0.0207(19) -0.0156(18) C68 0.082(3) 0.052(2) 0.069(3) -0.0168(19) 0.038(2) -0.0208(19) C69 0.082(4) 0.169(6) 0.142(5) -0.087(5) 0.060(4) -0.042(4) C70 0.069(3) 0.079(3) 0.176(6) -0.030(4) 0.046(4) -0.011(2) C71 0.082(3) 0.099(3) 0.123(4) 0.035(3) 0.031(3) 0.023(3) C72 0.080(3) 0.098(3) 0.090(3) 0.029(3) 0.039(2) 0.030(2) C73 0.062(2) 0.093(3) 0.067(2) -0.010(2) -0.0001(19) -0.018(2) C74 0.063(2) 0.098(3) 0.055(2) 0.010(2) 0.0102(18) 0.019(2) C102 0.0431(17) 0.0546(19) 0.0447(18) -0.0007(15) -0.0067(14) -0.0002(14) C103 0.0443(17) 0.0495(19) 0.0448(18) -0.0049(14) -0.0074(14) -0.0005(14) C104 0.0510(19) 0.0472(19) 0.0478(18) 0.0017(14) -0.0103(15) -0.0019(15) C105 0.057(2) 0.052(2) 0.0404(17) 0.0004(14) -0.0071(15) -0.0008(15) _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 C39 1.846(4) . ? Si1 C38 1.856(4) . ? Si1 C2 1.860(3) . ? Si1 C5 1.869(3) . ? Si2 C73 1.845(4) . ? Si2 C74 1.848(4) . ? Si2 C105 1.867(3) . ? Si2 C102 1.874(3) . ? N1 C10 1.337(4) . ? N1 C6 1.360(4) . ? N2 C15 1.326(4) . ? N2 C11 1.338(3) . ? N3 C32 1.337(4) . ? N3 C28 1.354(4) . ? N4 C33 1.325(4) . ? N4 C34 1.346(5) . ? N5 C67 1.336(4) . ? N5 C63 1.342(4) . ? N6 C68 1.323(4) . ? N6 C69 1.352(7) . ? N7 C41 1.331(4) . ? N7 C40 1.347(4) . ? N8 C45 1.331(5) . ? N8 C49 1.337(6) . ? C2 C3 1.355(4) . ? C2 C6 1.469(4) . ? C3 C16 1.489(4) . ? C3 C4 1.504(4) . ? C4 C5 1.349(4) . ? C4 C22 1.494(4) . ? C5 C28 1.458(4) . ? C6 C7 1.379(4) . ? C7 C8 1.366(4) . ? C7 H7 0.9300 . ? C8 C9 1.366(4) . ? C8 H8 0.9300 . ? C9 C10 1.377(4) . ? C9 H9 0.9300 . ? C10 C11 1.479(4) . ? C11 C12 1.367(4) . ? C12 C13 1.374(4) . ? C12 H12 0.9300 . ? C13 C14 1.364(4) . ? C13 H13 0.9300 . ? C14 C15 1.364(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C21 1.379(4) . ? C16 C17 1.378(4) . ? C17 C18 1.368(5) . ? C17 H17 0.9300 . ? C18 C19 1.371(5) . ? C18 H18 0.9300 . ? C19 C20 1.350(5) . ? C19 H19 0.9300 . ? C20 C21 1.374(5) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.372(4) . ? C22 C27 1.373(5) . ? C23 C24 1.368(5) . ? C23 H23 0.9300 . ? C24 C25 1.360(7) . ? C24 H24 0.9300 . ? C25 C26 1.355(7) . ? C25 H25 0.9300 . ? C26 C27 1.383(5) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.394(4) . ? C29 C30 1.368(5) . ? C29 H29 0.9300 . ? C30 C31 1.378(5) . ? C30 H30 0.9300 . ? C31 C32 1.382(4) . ? C31 H31 0.9300 . ? C32 C33 1.490(5) . ? C33 C37 1.370(5) . ? C34 C35 1.350(6) . ? C34 H34 0.9300 . ? C35 C36 1.358(6) . ? C35 H35 0.9300 . ? C36 C37 1.382(5) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C44 1.394(4) . ? C40 C102 1.467(4) . ? C41 C42 1.388(5) . ? C41 C45 1.490(5) . ? C42 C43 1.370(5) . ? C42 H42 0.9300 . ? C43 C44 1.371(4) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C46 1.379(5) . ? C46 C47 1.377(5) . ? C46 H46 0.9300 . ? C47 C48 1.371(8) . ? C47 H47 0.9300 . ? C48 C49 1.348(8) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C51 C56 1.380(4) . ? C51 C52 1.385(4) . ? C51 C103 1.488(4) . ? C52 C53 1.371(5) . ? C52 H52 0.9300 . ? C53 C54 1.357(6) . ? C53 H53 0.9300 . ? C54 C55 1.370(6) . ? C54 H54 0.9300 . ? C55 C56 1.384(5) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 C62 1.381(4) . ? C57 C58 1.385(4) . ? C57 C104 1.489(4) . ? C58 C59 1.378(4) . ? C58 H58 0.9300 . ? C59 C60 1.367(5) . ? C59 H59 0.9300 . ? C60 C61 1.365(5) . ? C60 H60 0.9300 . ? C61 C62 1.370(4) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 C64 1.385(4) . ? C63 C105 1.469(4) . ? C64 C65 1.370(5) . ? C64 H64 0.9300 . ? C65 C66 1.373(6) . ? C65 H65 0.9300 . ? C66 C67 1.378(5) . ? C66 H66 0.9300 . ? C67 C68 1.495(5) . ? C68 C72 1.360(5) . ? C69 C70 1.338(8) . ? C69 H69 0.9300 . ? C70 C71 1.345(6) . ? C70 H70 0.9300 . ? C71 C72 1.379(5) . ? C71 H71 0.9300 . ? C72 H72 0.9300 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C102 C103 1.359(4) . ? C103 C104 1.500(4) . ? C104 C105 1.362(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C39 Si1 C38 112.11(17) . . ? C39 Si1 C2 113.79(16) . . ? C38 Si1 C2 110.43(16) . . ? C39 Si1 C5 117.87(16) . . ? C38 Si1 C5 109.96(15) . . ? C2 Si1 C5 90.89(14) . . ? C73 Si2 C74 111.70(18) . . ? C73 Si2 C105 110.35(16) . . ? C74 Si2 C105 116.32(16) . . ? C73 Si2 C102 116.66(16) . . ? C74 Si2 C102 109.51(15) . . ? C105 Si2 C102 90.99(14) . . ? C10 N1 C6 118.6(3) . . ? C15 N2 C11 117.2(3) . . ? C32 N3 C28 119.4(3) . . ? C33 N4 C34 116.7(4) . . ? C67 N5 C63 118.8(3) . . ? C68 N6 C69 115.6(5) . . ? C41 N7 C40 119.1(3) . . ? C45 N8 C49 116.8(5) . . ? C3 C2 C6 126.9(3) . . ? C3 C2 Si1 109.2(2) . . ? C6 C2 Si1 123.8(2) . . ? C2 C3 C16 123.7(3) . . ? C2 C3 C4 114.8(3) . . ? C16 C3 C4 121.5(3) . . ? C5 C4 C22 126.4(3) . . ? C5 C4 C3 115.7(3) . . ? C22 C4 C3 117.6(3) . . ? C4 C5 C28 129.1(3) . . ? C4 C5 Si1 108.6(2) . . ? C28 C5 Si1 122.1(2) . . ? N1 C6 C7 120.8(3) . . ? N1 C6 C2 113.9(3) . . ? C7 C6 C2 125.2(3) . . ? C8 C7 C6 120.2(3) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 118.7(3) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C8 C9 C10 119.8(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? N1 C10 C9 121.9(3) . . ? N1 C10 C11 116.4(3) . . ? C9 C10 C11 121.7(3) . . ? N2 C11 C12 122.0(3) . . ? N2 C11 C10 116.5(3) . . ? C12 C11 C10 121.4(3) . . ? C11 C12 C13 119.6(3) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 118.8(3) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C15 C14 C13 118.0(3) . . ? C15 C14 H14 121.0 . . ? C13 C14 H14 121.0 . . ? N2 C15 C14 124.3(3) . . ? N2 C15 H15 117.8 . . ? C14 C15 H15 117.8 . . ? C21 C16 C17 117.8(3) . . ? C21 C16 C3 121.7(3) . . ? C17 C16 C3 120.3(3) . . ? C18 C17 C16 121.0(3) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 119.9(4) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 120.2(4) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 120.0(4) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C16 121.1(3) . . ? C20 C21 H21 119.4 . . ? C16 C21 H21 119.4 . . ? C23 C22 C27 117.8(3) . . ? C23 C22 C4 123.8(3) . . ? C27 C22 C4 118.4(3) . . ? C24 C23 C22 121.6(4) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C25 C24 C23 119.9(4) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 119.9(4) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.3(5) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C22 C27 C26 120.5(4) . . ? C22 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? N3 C28 C29 120.3(3) . . ? N3 C28 C5 113.9(3) . . ? C29 C28 C5 125.7(3) . . ? C30 C29 C28 119.9(3) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 119.3(3) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C30 C31 C32 118.8(3) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? N3 C32 C31 122.1(3) . . ? N3 C32 C33 117.6(3) . . ? C31 C32 C33 120.2(3) . . ? N4 C33 C37 122.5(4) . . ? N4 C33 C32 115.5(3) . . ? C37 C33 C32 122.0(3) . . ? N4 C34 C35 124.2(4) . . ? N4 C34 H34 117.9 . . ? C35 C34 H34 117.9 . . ? C34 C35 C36 118.8(4) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? C35 C36 C37 118.4(4) . . ? C35 C36 H36 120.8 . . ? C37 C36 H36 120.8 . . ? C33 C37 C36 119.4(4) . . ? C33 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? Si1 C38 H38A 109.5 . . ? Si1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si1 C39 H39A 109.5 . . ? Si1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N7 C40 C44 120.5(3) . . ? N7 C40 C102 114.3(3) . . ? C44 C40 C102 125.0(3) . . ? N7 C41 C42 122.8(3) . . ? N7 C41 C45 116.4(3) . . ? C42 C41 C45 120.7(3) . . ? C43 C42 C41 118.2(3) . . ? C43 C42 H42 120.9 . . ? C41 C42 H42 120.9 . . ? C42 C43 C44 119.6(3) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C43 C44 C40 119.7(3) . . ? C43 C44 H44 120.2 . . ? C40 C44 H44 120.2 . . ? N8 C45 C46 122.4(4) . . ? N8 C45 C41 116.4(4) . . ? C46 C45 C41 121.2(3) . . ? C47 C46 C45 119.4(5) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C48 C47 C46 118.1(6) . . ? C48 C47 H47 121.0 . . ? C46 C47 H47 121.0 . . ? C49 C48 C47 119.0(5) . . ? C49 C48 H48 120.5 . . ? C47 C48 H48 120.5 . . ? N8 C49 C48 124.4(6) . . ? N8 C49 H49 117.8 . . ? C48 C49 H49 117.8 . . ? C56 C51 C52 118.6(3) . . ? C56 C51 C103 120.4(3) . . ? C52 C51 C103 121.0(3) . . ? C53 C52 C51 120.8(4) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C54 C53 C52 120.2(4) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C55 120.3(4) . . ? C53 C54 H54 119.8 . . ? C55 C54 H54 119.8 . . ? C54 C55 C56 120.0(4) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C51 C56 C55 120.2(4) . . ? C51 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C62 C57 C58 118.3(3) . . ? C62 C57 C104 121.0(3) . . ? C58 C57 C104 120.6(3) . . ? C59 C58 C57 120.3(3) . . ? C59 C58 H58 119.9 . . ? C57 C58 H58 119.9 . . ? C60 C59 C58 120.4(3) . . ? C60 C59 H59 119.8 . . ? C58 C59 H59 119.8 . . ? C61 C60 C59 119.7(3) . . ? C61 C60 H60 120.1 . . ? C59 C60 H60 120.1 . . ? C60 C61 C62 120.3(3) . . ? C60 C61 H61 119.9 . . ? C62 C61 H61 119.9 . . ? C61 C62 C57 120.9(3) . . ? C61 C62 H62 119.5 . . ? C57 C62 H62 119.5 . . ? N5 C63 C64 121.4(3) . . ? N5 C63 C105 112.6(3) . . ? C64 C63 C105 126.0(3) . . ? C65 C64 C63 119.1(4) . . ? C65 C64 H64 120.5 . . ? C63 C64 H64 120.5 . . ? C64 C65 C66 119.8(4) . . ? C64 C65 H65 120.1 . . ? C66 C65 H65 120.1 . . ? C65 C66 C67 118.3(4) . . ? C65 C66 H66 120.8 . . ? C67 C66 H66 120.8 . . ? N5 C67 C66 122.6(4) . . ? N5 C67 C68 116.1(3) . . ? C66 C67 C68 121.3(4) . . ? N6 C68 C72 121.9(4) . . ? N6 C68 C67 116.3(4) . . ? C72 C68 C67 121.7(3) . . ? C70 C69 N6 125.8(5) . . ? C70 C69 H69 117.1 . . ? N6 C69 H69 117.1 . . ? C69 C70 C71 117.8(5) . . ? C69 C70 H70 121.1 . . ? C71 C70 H70 121.1 . . ? C70 C71 C72 118.5(5) . . ? C70 C71 H71 120.7 . . ? C72 C71 H71 120.7 . . ? C68 C72 C71 120.4(4) . . ? C68 C72 H72 119.8 . . ? C71 C72 H72 119.8 . . ? Si2 C73 H73A 109.5 . . ? Si2 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? Si2 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? Si2 C74 H74A 109.5 . . ? Si2 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? Si2 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C103 C102 C40 127.9(3) . . ? C103 C102 Si2 108.9(2) . . ? C40 C102 Si2 122.8(2) . . ? C102 C103 C51 125.6(3) . . ? C102 C103 C104 115.6(3) . . ? C51 C103 C104 118.8(3) . . ? C105 C104 C57 124.8(3) . . ? C105 C104 C103 115.2(3) . . ? C57 C104 C103 120.0(3) . . ? C104 C105 C63 129.2(3) . . ? C104 C105 Si2 109.2(2) . . ? C63 C105 Si2 121.2(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C39 Si1 C2 C3 -128.4(2) . . . . ? C38 Si1 C2 C3 104.5(3) . . . . ? C5 Si1 C2 C3 -7.3(3) . . . . ? C39 Si1 C2 C6 52.2(3) . . . . ? C38 Si1 C2 C6 -74.9(3) . . . . ? C5 Si1 C2 C6 173.3(3) . . . . ? C6 C2 C3 C16 4.4(5) . . . . ? Si1 C2 C3 C16 -175.0(3) . . . . ? C6 C2 C3 C4 -176.5(3) . . . . ? Si1 C2 C3 C4 4.1(3) . . . . ? C2 C3 C4 C5 3.0(4) . . . . ? C16 C3 C4 C5 -177.9(3) . . . . ? C2 C3 C4 C22 -171.0(3) . . . . ? C16 C3 C4 C22 8.0(4) . . . . ? C22 C4 C5 C28 -9.0(6) . . . . ? C3 C4 C5 C28 177.5(3) . . . . ? C22 C4 C5 Si1 165.1(3) . . . . ? C3 C4 C5 Si1 -8.4(3) . . . . ? C39 Si1 C5 C4 126.5(3) . . . . ? C38 Si1 C5 C4 -103.3(3) . . . . ? C2 Si1 C5 C4 8.8(3) . . . . ? C39 Si1 C5 C28 -58.9(3) . . . . ? C38 Si1 C5 C28 71.3(3) . . . . ? C2 Si1 C5 C28 -176.6(3) . . . . ? C10 N1 C6 C7 -2.3(5) . . . . ? C10 N1 C6 C2 -178.7(3) . . . . ? C3 C2 C6 N1 -147.3(3) . . . . ? Si1 C2 C6 N1 32.0(4) . . . . ? C3 C2 C6 C7 36.5(5) . . . . ? Si1 C2 C6 C7 -144.2(3) . . . . ? N1 C6 C7 C8 1.0(5) . . . . ? C2 C6 C7 C8 176.9(3) . . . . ? C6 C7 C8 C9 0.8(6) . . . . ? C7 C8 C9 C10 -1.2(6) . . . . ? C6 N1 C10 C9 1.9(5) . . . . ? C6 N1 C10 C11 179.8(3) . . . . ? C8 C9 C10 N1 -0.2(5) . . . . ? C8 C9 C10 C11 -177.9(3) . . . . ? C15 N2 C11 C12 -1.3(5) . . . . ? C15 N2 C11 C10 176.2(3) . . . . ? N1 C10 C11 N2 173.1(3) . . . . ? C9 C10 C11 N2 -9.1(5) . . . . ? N1 C10 C11 C12 -9.4(5) . . . . ? C9 C10 C11 C12 168.5(3) . . . . ? N2 C11 C12 C13 1.8(5) . . . . ? C10 C11 C12 C13 -175.6(3) . . . . ? C11 C12 C13 C14 -0.7(6) . . . . ? C12 C13 C14 C15 -0.9(6) . . . . ? C11 N2 C15 C14 -0.4(5) . . . . ? C13 C14 C15 N2 1.5(5) . . . . ? C2 C3 C16 C21 -116.8(4) . . . . ? C4 C3 C16 C21 64.2(4) . . . . ? C2 C3 C16 C17 58.8(5) . . . . ? C4 C3 C16 C17 -120.2(3) . . . . ? C21 C16 C17 C18 2.2(5) . . . . ? C3 C16 C17 C18 -173.7(3) . . . . ? C16 C17 C18 C19 -1.2(6) . . . . ? C17 C18 C19 C20 0.2(7) . . . . ? C18 C19 C20 C21 -0.3(7) . . . . ? C19 C20 C21 C16 1.3(6) . . . . ? C17 C16 C21 C20 -2.2(5) . . . . ? C3 C16 C21 C20 173.5(3) . . . . ? C5 C4 C22 C23 96.4(4) . . . . ? C3 C4 C22 C23 -90.2(4) . . . . ? C5 C4 C22 C27 -84.2(4) . . . . ? C3 C4 C22 C27 89.1(4) . . . . ? C27 C22 C23 C24 -0.6(6) . . . . ? C4 C22 C23 C24 178.8(3) . . . . ? C22 C23 C24 C25 1.3(7) . . . . ? C23 C24 C25 C26 -1.1(8) . . . . ? C24 C25 C26 C27 0.2(8) . . . . ? C23 C22 C27 C26 -0.4(6) . . . . ? C4 C22 C27 C26 -179.7(4) . . . . ? C25 C26 C27 C22 0.6(7) . . . . ? C32 N3 C28 C29 2.7(5) . . . . ? C32 N3 C28 C5 179.4(3) . . . . ? C4 C5 C28 N3 166.9(3) . . . . ? Si1 C5 C28 N3 -6.5(4) . . . . ? C4 C5 C28 C29 -16.6(6) . . . . ? Si1 C5 C28 C29 170.0(3) . . . . ? N3 C28 C29 C30 -2.1(5) . . . . ? C5 C28 C29 C30 -178.4(3) . . . . ? C28 C29 C30 C31 -0.8(6) . . . . ? C29 C30 C31 C32 2.9(6) . . . . ? C28 N3 C32 C31 -0.5(5) . . . . ? C28 N3 C32 C33 -177.6(3) . . . . ? C30 C31 C32 N3 -2.3(5) . . . . ? C30 C31 C32 C33 174.7(3) . . . . ? C34 N4 C33 C37 0.3(6) . . . . ? C34 N4 C33 C32 179.6(4) . . . . ? N3 C32 C33 N4 -178.9(3) . . . . ? C31 C32 C33 N4 4.0(5) . . . . ? N3 C32 C33 C37 0.4(5) . . . . ? C31 C32 C33 C37 -176.7(4) . . . . ? C33 N4 C34 C35 -0.3(7) . . . . ? N4 C34 C35 C36 1.0(8) . . . . ? C34 C35 C36 C37 -1.8(7) . . . . ? N4 C33 C37 C36 -1.2(6) . . . . ? C32 C33 C37 C36 179.6(4) . . . . ? C35 C36 C37 C33 1.9(7) . . . . ? C41 N7 C40 C44 -3.9(4) . . . . ? C41 N7 C40 C102 -179.9(3) . . . . ? C40 N7 C41 C42 3.1(4) . . . . ? C40 N7 C41 C45 -179.8(3) . . . . ? N7 C41 C42 C43 0.2(5) . . . . ? C45 C41 C42 C43 -176.8(3) . . . . ? C41 C42 C43 C44 -2.7(5) . . . . ? C42 C43 C44 C40 1.9(5) . . . . ? N7 C40 C44 C43 1.5(5) . . . . ? C102 C40 C44 C43 177.0(3) . . . . ? C49 N8 C45 C46 0.0(6) . . . . ? C49 N8 C45 C41 178.3(4) . . . . ? N7 C41 C45 N8 158.9(3) . . . . ? C42 C41 C45 N8 -23.9(5) . . . . ? N7 C41 C45 C46 -22.9(5) . . . . ? C42 C41 C45 C46 154.3(4) . . . . ? N8 C45 C46 C47 -0.3(6) . . . . ? C41 C45 C46 C47 -178.4(4) . . . . ? C45 C46 C47 C48 0.7(7) . . . . ? C46 C47 C48 C49 -0.9(9) . . . . ? C45 N8 C49 C48 -0.3(8) . . . . ? C47 C48 C49 N8 0.7(10) . . . . ? C56 C51 C52 C53 -0.1(5) . . . . ? C103 C51 C52 C53 179.2(3) . . . . ? C51 C52 C53 C54 0.6(6) . . . . ? C52 C53 C54 C55 -0.5(6) . . . . ? C53 C54 C55 C56 -0.1(6) . . . . ? C52 C51 C56 C55 -0.6(5) . . . . ? C103 C51 C56 C55 -179.9(3) . . . . ? C54 C55 C56 C51 0.7(6) . . . . ? C62 C57 C58 C59 -1.3(5) . . . . ? C104 C57 C58 C59 175.7(3) . . . . ? C57 C58 C59 C60 0.8(5) . . . . ? C58 C59 C60 C61 0.4(6) . . . . ? C59 C60 C61 C62 -1.1(6) . . . . ? C60 C61 C62 C57 0.5(6) . . . . ? C58 C57 C62 C61 0.7(5) . . . . ? C104 C57 C62 C61 -176.3(3) . . . . ? C67 N5 C63 C64 -1.3(5) . . . . ? C67 N5 C63 C105 -179.1(3) . . . . ? N5 C63 C64 C65 0.9(5) . . . . ? C105 C63 C64 C65 178.5(3) . . . . ? C63 C64 C65 C66 -0.1(6) . . . . ? C64 C65 C66 C67 -0.3(6) . . . . ? C63 N5 C67 C66 0.8(5) . . . . ? C63 N5 C67 C68 -180.0(3) . . . . ? C65 C66 C67 N5 -0.1(6) . . . . ? C65 C66 C67 C68 -179.2(3) . . . . ? C69 N6 C68 C72 1.0(6) . . . . ? C69 N6 C68 C67 -179.8(4) . . . . ? N5 C67 C68 N6 178.1(3) . . . . ? C66 C67 C68 N6 -2.7(5) . . . . ? N5 C67 C68 C72 -2.7(5) . . . . ? C66 C67 C68 C72 176.5(4) . . . . ? C68 N6 C69 C70 -0.8(8) . . . . ? N6 C69 C70 C71 0.1(9) . . . . ? C69 C70 C71 C72 0.5(8) . . . . ? N6 C68 C72 C71 -0.4(7) . . . . ? C67 C68 C72 C71 -179.6(4) . . . . ? C70 C71 C72 C68 -0.4(7) . . . . ? N7 C40 C102 C103 -151.1(3) . . . . ? C44 C40 C102 C103 33.2(5) . . . . ? N7 C40 C102 Si2 36.4(4) . . . . ? C44 C40 C102 Si2 -139.4(3) . . . . ? C73 Si2 C102 C103 114.9(2) . . . . ? C74 Si2 C102 C103 -117.0(2) . . . . ? C105 Si2 C102 C103 1.4(2) . . . . ? C73 Si2 C102 C40 -71.4(3) . . . . ? C74 Si2 C102 C40 56.7(3) . . . . ? C105 Si2 C102 C40 175.2(3) . . . . ? C40 C102 C103 C51 4.7(5) . . . . ? Si2 C102 C103 C51 178.1(3) . . . . ? C40 C102 C103 C104 -175.8(3) . . . . ? Si2 C102 C103 C104 -2.4(3) . . . . ? C56 C51 C103 C102 -120.3(4) . . . . ? C52 C51 C103 C102 60.4(5) . . . . ? C56 C51 C103 C104 60.1(4) . . . . ? C52 C51 C103 C104 -119.1(3) . . . . ? C62 C57 C104 C105 59.9(5) . . . . ? C58 C57 C104 C105 -117.1(4) . . . . ? C62 C57 C104 C103 -121.7(4) . . . . ? C58 C57 C104 C103 61.3(4) . . . . ? C102 C103 C104 C105 2.5(4) . . . . ? C51 C103 C104 C105 -177.9(3) . . . . ? C102 C103 C104 C57 -176.0(3) . . . . ? C51 C103 C104 C57 3.6(4) . . . . ? C57 C104 C105 C63 3.4(5) . . . . ? C103 C104 C105 C63 -175.1(3) . . . . ? C57 C104 C105 Si2 177.2(2) . . . . ? C103 C104 C105 Si2 -1.2(3) . . . . ? N5 C63 C105 C104 -160.4(3) . . . . ? C64 C63 C105 C104 21.9(5) . . . . ? N5 C63 C105 Si2 26.5(4) . . . . ? C64 C63 C105 Si2 -151.3(3) . . . . ? C73 Si2 C105 C104 -119.1(3) . . . . ? C74 Si2 C105 C104 112.4(2) . . . . ? C102 Si2 C105 C104 -0.1(2) . . . . ? C73 Si2 C105 C63 55.3(3) . . . . ? C74 Si2 C105 C63 -73.2(3) . . . . ? C102 Si2 C105 C63 174.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.42 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.259 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.046