# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Shaowu Wang' _publ_contact_author_address ;Anhui Laboratory of Molecule-Based Materials, School of Chemistry and Materials Science, Anhui Normal University, Wuhu, Anhui 241000, P. R. China. ; _publ_contact_author_email swwang@mail.ahnu.edu.cn _publ_contact_author_phone +86-553-5910015 _publ_contact_author_fax +86-553-3883517 loop_ _publ_author_name _publ_author_address 'Shuangliu Zhou' ;Anhui Laboratory of Molecule-Based Materials, School of Chemistry and Materials Science, Anhui Normal University, Wuhu, Anhui 241000, P. R. China. ; 'Shihong Wu' ;Anhui Laboratory of Molecule-Based Materials, School of Chemistry and Materials Science, Anhui Normal University, Wuhu, Anhui 241000, P. R. China. ; 'Hong Zhu' ;Anhui Laboratory of Molecule-Based Materials, School of Chemistry and Materials Science, Anhui Normal University, Wuhu, Anhui 241000, P. R. China. ; 'Shaowu Wang' ;Anhui Laboratory of Molecule-Based Materials, School of Chemistry and Materials Science, Anhui Normal University, Wuhu, Anhui 241000, P. R. China. ; data_3 _database_code_depnum_ccdc_archive 'CCDC 819827' #TrackingRef '4903_web_deposit_cif_file_0_ShuangliuZhou_1301667625.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H68 N6 Nd2 Si4' _chemical_formula_weight 1033.84 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' Nd Nd -0.1943 3.0179 '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 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 16.2452(11) _cell_length_b 13.0806(9) _cell_length_c 23.1275(16) _cell_angle_alpha 90.00 _cell_angle_beta 106.2000(10) _cell_angle_gamma 90.00 _cell_volume 4719.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 2.310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6948 _exptl_absorpt_correction_T_max 0.7533 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20017 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.58 _reflns_number_total 5442 _reflns_number_gt 4880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+5.7679P] 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 5442 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0671 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.145 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.036474(8) 0.701837(9) 0.186288(6) 0.03443(5) Uani 1 1 d . . . Si1 Si 0.04491(7) 0.79252(7) 0.04552(5) 0.0644(3) Uani 1 1 d . . . Si2 Si 0.17196(6) 0.63173(7) 0.09974(4) 0.0564(2) Uani 1 1 d . . . N3 N 0.08720(16) 0.70698(17) 0.10214(11) 0.0467(5) Uani 1 1 d . . . N1 N 0.08873(13) 0.81602(15) 0.29147(10) 0.0395(5) Uani 1 1 d . . . C16 C 0.1187(4) 0.9027(4) 0.0439(3) 0.140(3) Uani 1 1 d . . . H16A H 0.1054 0.9588 0.0665 0.210 Uiso 1 1 calc R . . H16B H 0.1112 0.9237 0.0029 0.210 Uiso 1 1 calc R . . H16C H 0.1770 0.8819 0.0613 0.210 Uiso 1 1 calc R . . C17 C 0.0157(4) 0.7402(5) -0.0319(2) 0.124(2) Uani 1 1 d . . . H17A H 0.0666 0.7185 -0.0418 0.186 Uiso 1 1 calc R . . H17B H -0.0126 0.7920 -0.0598 0.186 Uiso 1 1 calc R . . H17C H -0.0220 0.6829 -0.0344 0.186 Uiso 1 1 calc R . . C18 C -0.0551(4) 0.8471(5) 0.0567(3) 0.130(2) Uani 1 1 d . . . H18A H -0.0948 0.7930 0.0572 0.196 Uiso 1 1 calc R . . H18B H -0.0803 0.8935 0.0244 0.196 Uiso 1 1 calc R . . H18C H -0.0420 0.8832 0.0943 0.196 Uiso 1 1 calc R . . C19 C 0.1531(5) 0.5470(5) 0.0332(2) 0.147(3) Uani 1 1 d . . . H19A H 0.1013 0.5088 0.0289 0.221 Uiso 1 1 calc R . . H19B H 0.2005 0.5007 0.0384 0.221 Uiso 1 1 calc R . . H19C H 0.1478 0.5876 -0.0023 0.221 Uiso 1 1 calc R . . C20 C 0.2706(3) 0.7061(5) 0.1009(4) 0.136(3) Uani 1 1 d . . . H20A H 0.2590 0.7503 0.0664 0.204 Uiso 1 1 calc R . . H20B H 0.3160 0.6598 0.0998 0.204 Uiso 1 1 calc R . . H20C H 0.2875 0.7463 0.1370 0.204 Uiso 1 1 calc R . . C21 C 0.1992(3) 0.5465(3) 0.16617(19) 0.0888(13) Uani 1 1 d . . . H21A H 0.2090 0.5867 0.2022 0.133 Uiso 1 1 calc R . . H21B H 0.2500 0.5084 0.1670 0.133 Uiso 1 1 calc R . . H21C H 0.1526 0.5001 0.1639 0.133 Uiso 1 1 calc R . . C1 C 0.07283(17) 0.89426(19) 0.24942(13) 0.0466(6) Uani 1 1 d . . . C2 C 0.13336(19) 0.8949(2) 0.21810(15) 0.0550(7) Uani 1 1 d . . . H2 H 0.1343 0.9374 0.1861 0.066 Uiso 1 1 calc R . . C3 C 0.19432(19) 0.8179(2) 0.24426(15) 0.0515(7) Uani 1 1 d . . . H3 H 0.2430 0.8002 0.2328 0.062 Uiso 1 1 calc R . . C4 C 0.16658(16) 0.77487(19) 0.28998(13) 0.0411(5) Uani 1 1 d . . . C11 C 0.0000 0.9647(3) 0.2500 0.0583(11) Uani 1 2 d S . . C12 C -0.0258(3) 1.0332(3) 0.1939(2) 0.0870(13) Uani 1 1 d . . . H12A H -0.0417 0.9912 0.1584 0.130 Uiso 1 1 calc R . . H12B H 0.0218 1.0758 0.1926 0.130 Uiso 1 1 calc R . . H12C H -0.0735 1.0753 0.1955 0.130 Uiso 1 1 calc R . . N2 N 0.09100(12) 0.58840(15) 0.28680(9) 0.0363(4) Uani 1 1 d . . . C5 C 0.20801(17) 0.70189(19) 0.33982(13) 0.0446(6) Uani 1 1 d . . . C6 C 0.13744(16) 0.62840(19) 0.34157(12) 0.0407(5) Uani 1 1 d . . . C14 C 0.28264(19) 0.6431(3) 0.32756(17) 0.0636(8) Uani 1 1 d . . . H14A H 0.3074 0.5986 0.3609 0.095 Uiso 1 1 calc R . . H14B H 0.3253 0.6905 0.3226 0.095 Uiso 1 1 calc R . . H14C H 0.2622 0.6033 0.2915 0.095 Uiso 1 1 calc R . . C13 C 0.2429(2) 0.7613(3) 0.39861(15) 0.0648(9) Uani 1 1 d . . . H13A H 0.1984 0.8039 0.4055 0.097 Uiso 1 1 calc R . . H13B H 0.2901 0.8033 0.3957 0.097 Uiso 1 1 calc R . . H13C H 0.2620 0.7142 0.4314 0.097 Uiso 1 1 calc R . . C10 C 0.0000 0.4395(3) 0.2500 0.0415(8) Uani 1 2 d S . . C9 C 0.04323(16) 0.50948(18) 0.30093(12) 0.0390(5) Uani 1 1 d . . . C8 C 0.05237(19) 0.5072(2) 0.36182(13) 0.0511(7) Uani 1 1 d . . . H8 H 0.0243 0.4638 0.3819 0.061 Uiso 1 1 calc R . . C7 C 0.1132(2) 0.5842(2) 0.38807(13) 0.0530(7) Uani 1 1 d . . . H7 H 0.1327 0.6011 0.4287 0.064 Uiso 1 1 calc R . . C15 C 0.0673(2) 0.3702(2) 0.23440(16) 0.0577(8) Uani 1 1 d . . . H15A H 0.1119 0.4117 0.2267 0.087 Uiso 1 1 calc R . . H15B H 0.0406 0.3307 0.1992 0.087 Uiso 1 1 calc R . . H15C H 0.0914 0.3251 0.2675 0.087 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 Nd1 0.03279(8) 0.03531(8) 0.03533(8) 0.00262(5) 0.00975(5) -0.00127(5) Si1 0.0724(6) 0.0716(6) 0.0533(5) 0.0240(4) 0.0239(5) 0.0091(4) Si2 0.0603(5) 0.0706(5) 0.0433(4) 0.0073(4) 0.0229(4) 0.0112(4) N3 0.0507(13) 0.0520(13) 0.0413(12) 0.0090(9) 0.0189(10) 0.0007(10) N1 0.0333(10) 0.0342(10) 0.0476(12) -0.0010(8) 0.0059(9) -0.0005(8) C16 0.153(5) 0.108(4) 0.163(6) 0.077(4) 0.051(5) -0.018(4) C17 0.150(5) 0.150(5) 0.058(3) 0.018(3) 0.006(3) 0.034(4) C18 0.136(5) 0.145(5) 0.133(5) 0.083(4) 0.074(4) 0.088(4) C19 0.188(6) 0.160(6) 0.073(3) -0.039(3) 0.002(4) 0.087(5) C20 0.073(3) 0.155(6) 0.199(7) 0.073(5) 0.070(4) 0.018(3) C21 0.100(3) 0.094(3) 0.082(3) 0.038(2) 0.042(2) 0.043(2) C1 0.0405(13) 0.0330(11) 0.0590(16) 0.0015(11) 0.0016(12) -0.0062(10) C2 0.0505(16) 0.0480(15) 0.0630(18) 0.0089(13) 0.0100(13) -0.0163(13) C3 0.0382(14) 0.0512(15) 0.0656(19) -0.0025(13) 0.0152(13) -0.0130(12) C4 0.0302(12) 0.0379(12) 0.0523(15) -0.0043(11) 0.0065(10) -0.0045(9) C11 0.044(2) 0.0304(17) 0.090(3) 0.000 0.001(2) 0.000 C12 0.071(2) 0.0461(18) 0.129(4) 0.034(2) 0.003(2) -0.0022(16) N2 0.0324(10) 0.0349(10) 0.0411(11) 0.0018(8) 0.0093(8) 0.0018(8) C5 0.0323(12) 0.0442(14) 0.0504(16) -0.0028(11) -0.0002(11) 0.0015(10) C6 0.0349(12) 0.0398(12) 0.0425(13) 0.0023(10) 0.0025(10) 0.0035(10) C14 0.0358(14) 0.0642(19) 0.085(2) -0.0020(17) 0.0074(14) 0.0079(13) C13 0.0520(18) 0.0679(19) 0.0593(19) -0.0096(16) -0.0094(14) -0.0060(15) C10 0.0402(18) 0.0303(15) 0.055(2) 0.000 0.0152(16) 0.000 C9 0.0365(12) 0.0331(11) 0.0466(14) 0.0063(10) 0.0100(10) 0.0034(9) C8 0.0546(16) 0.0482(14) 0.0501(16) 0.0150(12) 0.0140(13) 0.0017(12) C7 0.0566(17) 0.0581(17) 0.0384(14) 0.0056(12) 0.0035(12) 0.0035(13) C15 0.0556(18) 0.0391(14) 0.082(2) -0.0012(14) 0.0246(16) 0.0092(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 N3 2.316(2) . ? Nd1 N1 2.686(2) 2 ? Nd1 N2 2.691(2) . ? Nd1 N2 2.756(2) 2 ? Nd1 N1 2.778(2) . ? Nd1 C4 2.881(3) . ? Nd1 C6 2.882(2) 2 ? Nd1 C9 2.882(2) 2 ? Nd1 C1 2.887(3) . ? Nd1 C2 2.959(3) . ? Nd1 C3 2.960(3) . ? Nd1 C7 2.984(3) 2 ? Si1 N3 1.714(2) . ? Si1 C17 1.852(5) . ? Si1 C18 1.858(5) . ? Si1 C16 1.882(5) . ? Si2 N3 1.706(3) . ? Si2 C21 1.849(4) . ? Si2 C19 1.852(5) . ? Si2 C20 1.869(5) . ? N1 C4 1.384(3) . ? N1 C1 1.386(3) . ? N1 Nd1 2.686(2) 2 ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C1 C2 1.374(4) . ? C1 C11 1.502(4) . ? C2 C3 1.424(4) . ? C2 H2 0.9300 . ? C3 C4 1.380(4) . ? C3 H3 0.9300 . ? C4 C5 1.503(4) . ? C11 C1 1.502(4) 2 ? C11 C12 1.536(4) 2 ? C11 C12 1.536(4) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? N2 C6 1.383(3) . ? N2 C9 1.384(3) . ? N2 Nd1 2.756(2) 2 ? C5 C6 1.505(4) . ? C5 C14 1.528(4) . ? C5 C13 1.531(4) . ? C6 C7 1.372(4) . ? C6 Nd1 2.882(2) 2 ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C10 C9 1.502(3) . ? C10 C9 1.502(3) 2 ? C10 C15 1.538(3) 2 ? C10 C15 1.538(3) . ? C9 C8 1.374(4) . ? C9 Nd1 2.882(2) 2 ? C8 C7 1.423(4) . ? C8 Nd1 2.984(3) 2 ? C8 H8 0.9300 . ? C7 Nd1 2.984(3) 2 ? C7 H7 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? 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 N3 Nd1 N1 127.63(8) . 2 ? N3 Nd1 N2 129.30(7) . . ? N1 Nd1 N2 103.03(6) 2 . ? N3 Nd1 N2 132.16(7) . 2 ? N1 Nd1 N2 66.38(6) 2 2 ? N2 Nd1 N2 66.11(8) . 2 ? N3 Nd1 N1 128.81(8) . . ? N1 Nd1 N1 66.18(8) 2 . ? N2 Nd1 N1 66.01(6) . . ? N2 Nd1 N1 99.03(6) 2 . ? N3 Nd1 C4 109.84(8) . . ? N1 Nd1 C4 94.31(7) 2 . ? N2 Nd1 C4 58.37(7) . . ? N2 Nd1 C4 114.42(7) 2 . ? N1 Nd1 C4 28.23(7) . . ? N3 Nd1 C6 112.23(8) . 2 ? N1 Nd1 C6 58.71(7) 2 2 ? N2 Nd1 C6 94.31(7) . 2 ? N2 Nd1 C6 28.30(7) 2 2 ? N1 Nd1 C6 114.58(7) . 2 ? C4 Nd1 C6 137.93(8) . 2 ? N3 Nd1 C9 112.76(8) . 2 ? N1 Nd1 C9 94.58(7) 2 2 ? N2 Nd1 C9 58.61(7) . 2 ? N2 Nd1 C9 28.31(6) 2 2 ? N1 Nd1 C9 114.57(7) . 2 ? C4 Nd1 C9 116.76(7) . 2 ? C6 Nd1 C9 44.89(7) 2 2 ? N3 Nd1 C1 109.21(8) . . ? N1 Nd1 C1 58.49(7) 2 . ? N2 Nd1 C1 94.14(7) . . ? N2 Nd1 C1 114.57(7) 2 . ? N1 Nd1 C1 28.23(7) . . ? C4 Nd1 C1 44.85(7) . . ? C6 Nd1 C1 116.94(8) 2 . ? C9 Nd1 C1 138.03(8) 2 . ? N3 Nd1 C2 83.96(9) . . ? N1 Nd1 C2 81.74(8) 2 . ? N2 Nd1 C2 103.41(7) . . ? N2 Nd1 C2 141.68(8) 2 . ? N1 Nd1 C2 46.51(8) . . ? C4 Nd1 C2 45.10(8) . . ? C6 Nd1 C2 139.51(8) 2 . ? C9 Nd1 C2 160.53(8) 2 . ? C1 Nd1 C2 27.16(8) . . ? N3 Nd1 C3 84.22(9) . . ? N1 Nd1 C3 103.57(8) 2 . ? N2 Nd1 C3 81.77(7) . . ? N2 Nd1 C3 141.67(8) 2 . ? N1 Nd1 C3 46.61(8) . . ? C4 Nd1 C3 27.29(8) . . ? C6 Nd1 C3 160.69(8) 2 . ? C9 Nd1 C3 139.34(8) 2 . ? C1 Nd1 C3 45.13(8) . . ? C2 Nd1 C3 27.84(8) . . ? N3 Nd1 C7 87.40(9) . 2 ? N1 Nd1 C7 81.85(8) 2 2 ? N2 Nd1 C7 103.43(7) . 2 ? N2 Nd1 C7 46.34(7) 2 2 ? N1 Nd1 C7 141.51(8) . 2 ? C4 Nd1 C7 160.24(8) . 2 ? C6 Nd1 C7 26.98(8) 2 2 ? C9 Nd1 C7 44.91(8) 2 2 ? C1 Nd1 C7 139.45(8) . 2 ? C2 Nd1 C7 151.05(8) . 2 ? C3 Nd1 C7 171.61(9) . 2 ? N3 Si1 C17 116.0(2) . . ? N3 Si1 C18 108.91(17) . . ? C17 Si1 C18 106.2(3) . . ? N3 Si1 C16 113.2(2) . . ? C17 Si1 C16 104.9(3) . . ? C18 Si1 C16 107.1(3) . . ? N3 Si2 C21 109.20(15) . . ? N3 Si2 C19 115.1(2) . . ? C21 Si2 C19 106.0(3) . . ? N3 Si2 C20 113.3(2) . . ? C21 Si2 C20 107.3(3) . . ? C19 Si2 C20 105.4(4) . . ? Si2 N3 Si1 120.46(14) . . ? Si2 N3 Nd1 119.35(12) . . ? Si1 N3 Nd1 120.02(13) . . ? C4 N1 C1 105.2(2) . . ? C4 N1 Nd1 122.32(15) . 2 ? C1 N1 Nd1 122.84(16) . 2 ? C4 N1 Nd1 80.04(14) . . ? C1 N1 Nd1 80.26(15) . . ? Nd1 N1 Nd1 78.82(5) 2 . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si1 C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C2 C1 N1 110.7(2) . . ? C2 C1 C11 133.0(2) . . ? N1 C1 C11 116.1(2) . . ? C2 C1 Nd1 79.32(17) . . ? N1 C1 Nd1 71.51(14) . . ? C11 C1 Nd1 119.25(16) . . ? C1 C2 C3 106.6(3) . . ? C1 C2 Nd1 73.52(15) . . ? C3 C2 Nd1 76.13(16) . . ? C1 C2 H2 126.7 . . ? C3 C2 H2 126.7 . . ? Nd1 C2 H2 116.0 . . ? C4 C3 C2 106.1(3) . . ? C4 C3 Nd1 73.19(15) . . ? C2 C3 Nd1 76.03(16) . . ? C4 C3 H3 127.0 . . ? C2 C3 H3 127.0 . . ? Nd1 C3 H3 116.2 . . ? C3 C4 N1 110.9(2) . . ? C3 C4 C5 132.4(3) . . ? N1 C4 C5 116.4(2) . . ? C3 C4 Nd1 79.52(17) . . ? N1 C4 Nd1 71.73(14) . . ? C5 C4 Nd1 119.68(16) . . ? C1 C11 C1 104.4(3) 2 . ? C1 C11 C12 112.3(2) 2 2 ? C1 C11 C12 109.60(18) . 2 ? C1 C11 C12 109.60(18) 2 . ? C1 C11 C12 112.3(2) . . ? C12 C11 C12 108.7(4) 2 . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 N2 C9 105.3(2) . . ? C6 N2 Nd1 123.12(15) . . ? C9 N2 Nd1 122.96(15) . . ? C6 N2 Nd1 80.90(14) . 2 ? C9 N2 Nd1 80.92(13) . 2 ? Nd1 N2 Nd1 79.12(5) . 2 ? C4 C5 C6 104.2(2) . . ? C4 C5 C14 112.7(3) . . ? C6 C5 C14 109.5(2) . . ? C4 C5 C13 109.5(2) . . ? C6 C5 C13 113.4(3) . . ? C14 C5 C13 107.7(2) . . ? C7 C6 N2 110.8(2) . . ? C7 C6 C5 132.6(3) . . ? N2 C6 C5 116.2(2) . . ? C7 C6 Nd1 80.68(17) . 2 ? N2 C6 Nd1 70.80(13) . 2 ? C5 C6 Nd1 119.19(16) . 2 ? C5 C14 H14A 109.5 . . ? C5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C5 C13 H13A 109.5 . . ? C5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C10 C9 104.9(3) . 2 ? C9 C10 C15 112.48(16) . 2 ? C9 C10 C15 109.60(16) 2 2 ? C9 C10 C15 109.60(16) . . ? C9 C10 C15 112.48(16) 2 . ? C15 C10 C15 107.8(3) 2 . ? C8 C9 N2 110.5(2) . . ? C8 C9 C10 133.1(2) . . ? N2 C9 C10 116.1(2) . . ? C8 C9 Nd1 80.62(16) . 2 ? N2 C9 Nd1 70.77(12) . 2 ? C10 C9 Nd1 119.15(15) . 2 ? C9 C8 C7 106.6(2) . . ? C9 C8 Nd1 72.35(15) . 2 ? C7 C8 Nd1 76.21(16) . 2 ? C9 C8 H8 126.7 . . ? C7 C8 H8 126.7 . . ? Nd1 C8 H8 116.9 2 . ? C6 C7 C8 106.3(2) . . ? C6 C7 Nd1 72.34(15) . 2 ? C8 C7 Nd1 76.21(16) . 2 ? C6 C7 H7 126.8 . . ? C8 C7 H7 126.8 . . ? Nd1 C7 H7 116.9 2 . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Si2 N3 Si1 -178.4(2) . . . . ? C19 Si2 N3 Si1 -59.4(3) . . . . ? C20 Si2 N3 Si1 62.1(3) . . . . ? C21 Si2 N3 Nd1 6.4(2) . . . . ? C19 Si2 N3 Nd1 125.5(3) . . . . ? C20 Si2 N3 Nd1 -113.1(3) . . . . ? C17 Si1 N3 Si2 52.2(3) . . . . ? C18 Si1 N3 Si2 171.8(3) . . . . ? C16 Si1 N3 Si2 -69.1(3) . . . . ? C17 Si1 N3 Nd1 -132.7(3) . . . . ? C18 Si1 N3 Nd1 -13.0(3) . . . . ? C16 Si1 N3 Nd1 106.1(3) . . . . ? N1 Nd1 N3 Si2 176.28(11) 2 . . . ? N2 Nd1 N3 Si2 -0.82(19) . . . . ? N2 Nd1 N3 Si2 -92.83(16) 2 . . . ? N1 Nd1 N3 Si2 88.26(15) . . . . ? C4 Nd1 N3 Si2 64.02(15) . . . . ? C6 Nd1 N3 Si2 -116.88(14) 2 . . . ? C9 Nd1 N3 Si2 -68.07(16) 2 . . . ? C1 Nd1 N3 Si2 111.76(14) . . . . ? C2 Nd1 N3 Si2 101.58(15) . . . . ? C3 Nd1 N3 Si2 73.59(15) . . . . ? C7 Nd1 N3 Si2 -106.09(15) 2 . . . ? N1 Nd1 N3 Si1 1.08(19) 2 . . . ? N2 Nd1 N3 Si1 -176.02(11) . . . . ? N2 Nd1 N3 Si1 91.97(15) 2 . . . ? N1 Nd1 N3 Si1 -86.94(16) . . . . ? C4 Nd1 N3 Si1 -111.18(14) . . . . ? C6 Nd1 N3 Si1 67.91(15) 2 . . . ? C9 Nd1 N3 Si1 116.72(14) 2 . . . ? C1 Nd1 N3 Si1 -63.44(16) . . . . ? C2 Nd1 N3 Si1 -73.62(15) . . . . ? C3 Nd1 N3 Si1 -101.61(15) . . . . ? C7 Nd1 N3 Si1 78.71(15) 2 . . . ? N3 Nd1 N1 C4 -54.73(17) . . . . ? N1 Nd1 N1 C4 -174.82(16) 2 . . . ? N2 Nd1 N1 C4 67.39(14) . . . . ? N2 Nd1 N1 C4 126.08(15) 2 . . . ? C6 Nd1 N1 C4 150.89(14) 2 . . . ? C9 Nd1 N1 C4 101.25(15) 2 . . . ? C1 Nd1 N1 C4 -107.5(2) . . . . ? C2 Nd1 N1 C4 -73.14(16) . . . . ? C3 Nd1 N1 C4 -34.44(15) . . . . ? C7 Nd1 N1 C4 148.70(15) 2 . . . ? N3 Nd1 N1 C1 52.75(18) . . . . ? N1 Nd1 N1 C1 -67.34(13) 2 . . . ? N2 Nd1 N1 C1 174.87(16) . . . . ? N2 Nd1 N1 C1 -126.43(15) 2 . . . ? C4 Nd1 N1 C1 107.5(2) . . . . ? C6 Nd1 N1 C1 -101.62(15) 2 . . . ? C9 Nd1 N1 C1 -151.26(15) 2 . . . ? C2 Nd1 N1 C1 34.34(15) . . . . ? C3 Nd1 N1 C1 73.04(17) . . . . ? C7 Nd1 N1 C1 -103.82(18) 2 . . . ? N3 Nd1 N1 Nd1 179.25(7) . . . 2 ? N1 Nd1 N1 Nd1 59.16(7) 2 . . 2 ? N2 Nd1 N1 Nd1 -58.63(6) . . . 2 ? N2 Nd1 N1 Nd1 0.07(6) 2 . . 2 ? C4 Nd1 N1 Nd1 -126.02(16) . . . 2 ? C6 Nd1 N1 Nd1 24.88(8) 2 . . 2 ? C9 Nd1 N1 Nd1 -24.77(8) 2 . . 2 ? C1 Nd1 N1 Nd1 126.50(16) . . . 2 ? C2 Nd1 N1 Nd1 160.84(11) . . . 2 ? C3 Nd1 N1 Nd1 -160.46(11) . . . 2 ? C7 Nd1 N1 Nd1 22.68(13) 2 . . 2 ? C4 N1 C1 C2 6.4(3) . . . . ? Nd1 N1 C1 C2 -140.2(2) 2 . . . ? Nd1 N1 C1 C2 -70.4(2) . . . . ? C4 N1 C1 C11 -169.0(2) . . . . ? Nd1 N1 C1 C11 44.4(3) 2 . . . ? Nd1 N1 C1 C11 114.2(2) . . . . ? C4 N1 C1 Nd1 76.79(16) . . . . ? Nd1 N1 C1 Nd1 -69.82(14) 2 . . . ? N3 Nd1 C1 C2 -22.64(19) . . . . ? N1 Nd1 C1 C2 -145.6(2) 2 . . . ? N2 Nd1 C1 C2 111.60(17) . . . . ? N2 Nd1 C1 C2 177.18(16) 2 . . . ? N1 Nd1 C1 C2 116.3(2) . . . . ? C4 Nd1 C1 C2 76.52(18) . . . . ? C6 Nd1 C1 C2 -151.43(16) 2 . . . ? C9 Nd1 C1 C2 157.13(16) 2 . . . ? C3 Nd1 C1 C2 37.54(17) . . . . ? C7 Nd1 C1 C2 -132.11(18) 2 . . . ? N3 Nd1 C1 N1 -138.94(15) . . . . ? N1 Nd1 C1 N1 98.06(15) 2 . . . ? N2 Nd1 C1 N1 -4.70(15) . . . . ? N2 Nd1 C1 N1 60.89(16) 2 . . . ? C4 Nd1 C1 N1 -39.77(14) . . . . ? C6 Nd1 C1 N1 92.28(15) 2 . . . ? C9 Nd1 C1 N1 40.84(19) 2 . . . ? C2 Nd1 C1 N1 -116.3(2) . . . . ? C3 Nd1 C1 N1 -78.75(16) . . . . ? C7 Nd1 C1 N1 111.60(16) 2 . . . ? N3 Nd1 C1 C11 110.95(19) . . . . ? N1 Nd1 C1 C11 -12.06(16) 2 . . . ? N2 Nd1 C1 C11 -114.82(18) . . . . ? N2 Nd1 C1 C11 -49.2(2) 2 . . . ? N1 Nd1 C1 C11 -110.1(3) . . . . ? C4 Nd1 C1 C11 -149.9(2) . . . . ? C6 Nd1 C1 C11 -17.8(2) 2 . . . ? C9 Nd1 C1 C11 -69.3(2) 2 . . . ? C2 Nd1 C1 C11 133.6(3) . . . . ? C3 Nd1 C1 C11 171.1(2) . . . . ? C7 Nd1 C1 C11 1.5(3) 2 . . . ? N1 C1 C2 C3 -4.2(3) . . . . ? C11 C1 C2 C3 170.2(3) . . . . ? Nd1 C1 C2 C3 -69.5(2) . . . . ? N1 C1 C2 Nd1 65.38(18) . . . . ? C11 C1 C2 Nd1 -120.3(3) . . . . ? N3 Nd1 C2 C1 158.56(18) . . . . ? N1 Nd1 C2 C1 29.08(17) 2 . . . ? N2 Nd1 C2 C1 -72.43(17) . . . . ? N2 Nd1 C2 C1 -4.1(2) 2 . . . ? N1 Nd1 C2 C1 -35.77(15) . . . . ? C4 Nd1 C2 C1 -75.49(18) . . . . ? C6 Nd1 C2 C1 41.0(2) 2 . . . ? C9 Nd1 C2 C1 -51.2(3) 2 . . . ? C3 Nd1 C2 C1 -112.4(3) . . . . ? C7 Nd1 C2 C1 85.2(2) 2 . . . ? N3 Nd1 C2 C3 -89.1(2) . . . . ? N1 Nd1 C2 C3 141.5(2) 2 . . . ? N2 Nd1 C2 C3 40.0(2) . . . . ? N2 Nd1 C2 C3 108.3(2) 2 . . . ? N1 Nd1 C2 C3 76.61(19) . . . . ? C4 Nd1 C2 C3 36.89(18) . . . . ? C6 Nd1 C2 C3 153.43(17) 2 . . . ? C9 Nd1 C2 C3 61.2(3) 2 . . . ? C1 Nd1 C2 C3 112.4(3) . . . . ? C7 Nd1 C2 C3 -162.46(19) 2 . . . ? C1 C2 C3 C4 0.2(3) . . . . ? Nd1 C2 C3 C4 -67.54(19) . . . . ? C1 C2 C3 Nd1 67.7(2) . . . . ? N3 Nd1 C3 C4 -160.05(18) . . . . ? N1 Nd1 C3 C4 72.58(17) 2 . . . ? N2 Nd1 C3 C4 -28.92(16) . . . . ? N2 Nd1 C3 C4 3.6(2) 2 . . . ? N1 Nd1 C3 C4 35.70(15) . . . . ? C6 Nd1 C3 C4 50.5(3) 2 . . . ? C9 Nd1 C3 C4 -41.4(2) 2 . . . ? C1 Nd1 C3 C4 75.38(19) . . . . ? C2 Nd1 C3 C4 111.9(3) . . . . ? C7 Nd1 C3 C4 -157.8(5) 2 . . . ? N3 Nd1 C3 C2 88.00(19) . . . . ? N1 Nd1 C3 C2 -39.4(2) 2 . . . ? N2 Nd1 C3 C2 -140.9(2) . . . . ? N2 Nd1 C3 C2 -108.3(2) 2 . . . ? N1 Nd1 C3 C2 -76.24(19) . . . . ? C4 Nd1 C3 C2 -111.9(3) . . . . ? C6 Nd1 C3 C2 -61.4(3) 2 . . . ? C9 Nd1 C3 C2 -153.38(17) 2 . . . ? C1 Nd1 C3 C2 -36.56(18) . . . . ? C7 Nd1 C3 C2 90.2(6) 2 . . . ? C2 C3 C4 N1 3.9(3) . . . . ? Nd1 C3 C4 N1 -65.68(18) . . . . ? C2 C3 C4 C5 -169.6(3) . . . . ? Nd1 C3 C4 C5 120.9(3) . . . . ? C2 C3 C4 Nd1 69.5(2) . . . . ? C1 N1 C4 C3 -6.3(3) . . . . ? Nd1 N1 C4 C3 140.55(19) 2 . . . ? Nd1 N1 C4 C3 70.7(2) . . . . ? C1 N1 C4 C5 168.3(2) . . . . ? Nd1 N1 C4 C5 -44.9(3) 2 . . . ? Nd1 N1 C4 C5 -114.7(2) . . . . ? C1 N1 C4 Nd1 -76.95(17) . . . . ? Nd1 N1 C4 Nd1 69.87(14) 2 . . . ? N3 Nd1 C4 C3 21.15(19) . . . . ? N1 Nd1 C4 C3 -111.54(17) 2 . . . ? N2 Nd1 C4 C3 145.80(19) . . . . ? N2 Nd1 C4 C3 -177.52(16) 2 . . . ? N1 Nd1 C4 C3 -116.3(2) . . . . ? C6 Nd1 C4 C3 -157.60(16) 2 . . . ? C9 Nd1 C4 C3 151.12(16) 2 . . . ? C1 Nd1 C4 C3 -76.51(19) . . . . ? C2 Nd1 C4 C3 -37.70(17) . . . . ? C7 Nd1 C4 C3 170.6(2) 2 . . . ? N3 Nd1 C4 N1 137.44(14) . . . . ? N1 Nd1 C4 N1 4.75(15) 2 . . . ? N2 Nd1 C4 N1 -97.91(16) . . . . ? N2 Nd1 C4 N1 -61.23(15) 2 . . . ? C6 Nd1 C4 N1 -41.31(19) 2 . . . ? C9 Nd1 C4 N1 -92.59(15) 2 . . . ? C1 Nd1 C4 N1 39.78(14) . . . . ? C2 Nd1 C4 N1 78.59(16) . . . . ? C3 Nd1 C4 N1 116.3(2) . . . . ? C7 Nd1 C4 N1 -73.1(3) 2 . . . ? N3 Nd1 C4 C5 -112.0(2) . . . . ? N1 Nd1 C4 C5 115.3(2) 2 . . . ? N2 Nd1 C4 C5 12.62(18) . . . . ? N2 Nd1 C4 C5 49.3(2) 2 . . . ? N1 Nd1 C4 C5 110.5(3) . . . . ? C6 Nd1 C4 C5 69.2(2) 2 . . . ? C9 Nd1 C4 C5 17.9(2) 2 . . . ? C1 Nd1 C4 C5 150.3(3) . . . . ? C2 Nd1 C4 C5 -170.9(3) . . . . ? C3 Nd1 C4 C5 -133.2(3) . . . . ? C7 Nd1 C4 C5 37.5(4) 2 . . . ? C2 C1 C11 C1 137.3(4) . . . 2 ? N1 C1 C11 C1 -48.62(16) . . . 2 ? Nd1 C1 C11 C1 33.87(8) . . . 2 ? C2 C1 C11 C12 -102.3(4) . . . 2 ? N1 C1 C11 C12 71.8(3) . . . 2 ? Nd1 C1 C11 C12 154.3(2) . . . 2 ? C2 C1 C11 C12 18.6(4) . . . . ? N1 C1 C11 C12 -167.3(2) . . . . ? Nd1 C1 C11 C12 -84.8(3) . . . . ? N3 Nd1 N2 C6 106.23(19) . . . . ? N1 Nd1 N2 C6 -71.41(19) 2 . . . ? N2 Nd1 N2 C6 -127.9(2) 2 . . . ? N1 Nd1 N2 C6 -15.25(18) . . . . ? C4 Nd1 N2 C6 15.60(18) . . . . ? C6 Nd1 N2 C6 -130.27(17) 2 . . . ? C9 Nd1 N2 C6 -158.8(2) 2 . . . ? C1 Nd1 N2 C6 -12.82(19) . . . . ? C2 Nd1 N2 C6 13.1(2) . . . . ? C3 Nd1 N2 C6 30.70(19) . . . . ? C7 Nd1 N2 C6 -156.00(18) 2 . . . ? N3 Nd1 N2 C9 -110.71(19) . . . . ? N1 Nd1 N2 C9 71.64(19) 2 . . . ? N2 Nd1 N2 C9 15.17(17) 2 . . . ? N1 Nd1 N2 C9 127.81(19) . . . . ? C4 Nd1 N2 C9 158.7(2) . . . . ? C6 Nd1 N2 C9 12.78(19) 2 . . . ? C9 Nd1 N2 C9 -15.77(19) 2 . . . ? C1 Nd1 N2 C9 130.24(19) . . . . ? C2 Nd1 N2 C9 156.11(18) . . . . ? C3 Nd1 N2 C9 173.75(19) . . . . ? C7 Nd1 N2 C9 -12.9(2) 2 . . . ? N3 Nd1 N2 Nd1 177.71(8) . . . 2 ? N1 Nd1 N2 Nd1 0.07(6) 2 . . 2 ? N2 Nd1 N2 Nd1 -56.41(6) 2 . . 2 ? N1 Nd1 N2 Nd1 56.24(6) . . . 2 ? C4 Nd1 N2 Nd1 87.09(8) . . . 2 ? C6 Nd1 N2 Nd1 -58.79(6) 2 . . 2 ? C9 Nd1 N2 Nd1 -87.35(7) 2 . . 2 ? C1 Nd1 N2 Nd1 58.67(7) . . . 2 ? C2 Nd1 N2 Nd1 84.54(8) . . . 2 ? C3 Nd1 N2 Nd1 102.18(7) . . . 2 ? C7 Nd1 N2 Nd1 -84.52(7) 2 . . 2 ? C3 C4 C5 C6 -137.8(3) . . . . ? N1 C4 C5 C6 49.0(3) . . . . ? Nd1 C4 C5 C6 -34.1(3) . . . . ? C3 C4 C5 C14 -19.2(4) . . . . ? N1 C4 C5 C14 167.6(2) . . . . ? Nd1 C4 C5 C14 84.5(3) . . . . ? C3 C4 C5 C13 100.7(4) . . . . ? N1 C4 C5 C13 -72.5(3) . . . . ? Nd1 C4 C5 C13 -155.6(2) . . . . ? C9 N2 C6 C7 -6.3(3) . . . . ? Nd1 N2 C6 C7 142.15(19) . . . . ? Nd1 N2 C6 C7 71.6(2) 2 . . . ? C9 N2 C6 C5 168.3(2) . . . . ? Nd1 N2 C6 C5 -43.3(3) . . . . ? Nd1 N2 C6 C5 -113.8(2) 2 . . . ? C9 N2 C6 Nd1 -77.90(15) . . . 2 ? Nd1 N2 C6 Nd1 70.57(13) . . . 2 ? C4 C5 C6 C7 -139.0(3) . . . . ? C14 C5 C6 C7 100.2(4) . . . . ? C13 C5 C6 C7 -20.0(4) . . . . ? C4 C5 C6 N2 47.9(3) . . . . ? C14 C5 C6 N2 -72.9(3) . . . . ? C13 C5 C6 N2 166.9(2) . . . . ? C4 C5 C6 Nd1 -33.8(3) . . . 2 ? C14 C5 C6 Nd1 -154.5(2) . . . 2 ? C13 C5 C6 Nd1 85.2(3) . . . 2 ? C6 N2 C9 C8 6.2(3) . . . . ? Nd1 N2 C9 C8 -142.30(18) . . . . ? Nd1 N2 C9 C8 -71.7(2) 2 . . . ? C6 N2 C9 C10 -168.31(19) . . . . ? Nd1 N2 C9 C10 43.2(3) . . . . ? Nd1 N2 C9 C10 113.81(18) 2 . . . ? C6 N2 C9 Nd1 77.89(15) . . . 2 ? Nd1 N2 C9 Nd1 -70.65(12) . . . 2 ? C9 C10 C9 C8 139.2(3) 2 . . . ? C15 C10 C9 C8 20.1(4) 2 . . . ? C15 C10 C9 C8 -99.8(3) . . . . ? C9 C10 C9 N2 -47.85(15) 2 . . . ? C15 C10 C9 N2 -166.9(2) 2 . . . ? C15 C10 C9 N2 73.2(3) . . . . ? C9 C10 C9 Nd1 33.70(7) 2 . . 2 ? C15 C10 C9 Nd1 -85.4(2) 2 . . 2 ? C15 C10 C9 Nd1 154.70(18) . . . 2 ? N2 C9 C8 C7 -3.9(3) . . . . ? C10 C9 C8 C7 169.4(3) . . . . ? Nd1 C9 C8 C7 -69.2(2) 2 . . . ? N2 C9 C8 Nd1 65.28(17) . . . 2 ? C10 C9 C8 Nd1 -121.4(3) . . . 2 ? N2 C6 C7 C8 4.0(3) . . . . ? C5 C6 C7 C8 -169.3(3) . . . . ? Nd1 C6 C7 C8 69.3(2) 2 . . . ? N2 C6 C7 Nd1 -65.23(17) . . . 2 ? C5 C6 C7 Nd1 121.4(3) . . . 2 ? C9 C8 C7 C6 -0.1(3) . . . . ? Nd1 C8 C7 C6 -66.6(2) 2 . . . ? C9 C8 C7 Nd1 66.49(19) . . . 2 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.487 _refine_diff_density_min -1.059 _refine_diff_density_rms 0.149 # Attachment '4904_web_deposit_cif_file_1_ShuangliuZhou_1301667625.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 819828' #TrackingRef '4904_web_deposit_cif_file_1_ShuangliuZhou_1301667625.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H68 N6 Si4 Sm2' _chemical_formula_weight 1046.06 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' Sm Sm -0.1638 3.4418 '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 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 16.2516(9) _cell_length_b 13.0822(7) _cell_length_c 23.0260(13) _cell_angle_alpha 90.00 _cell_angle_beta 106.0490(10) _cell_angle_gamma 90.00 _cell_volume 4704.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 2.607 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6958 _exptl_absorpt_correction_T_max 0.7450 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19997 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.57 _reflns_number_total 5429 _reflns_number_gt 4724 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+5.4044P] 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 5429 _refine_ls_number_parameters 246 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_ref 0.0610 _refine_ls_wR_factor_gt 0.0572 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.125 _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 Sm1 Sm 0.036672(8) 0.203044(10) 0.186949(6) 0.03697(5) Uani 1 1 d . . . Si1 Si 0.17171(6) 0.13237(8) 0.10083(4) 0.0590(2) Uani 1 1 d U . . Si2 Si 0.04519(7) 0.29252(8) 0.04611(5) 0.0676(3) Uani 1 1 d U . . N3 N 0.08677(17) 0.20779(18) 0.10350(11) 0.0495(6) Uani 1 1 d . . . N1 N 0.08794(14) 0.31621(16) 0.29130(11) 0.0426(5) Uani 1 1 d . . . C16 C 0.1997(3) 0.0471(4) 0.16723(19) 0.0906(13) Uani 1 1 d U . . H16A H 0.2000 0.0855 0.2028 0.136 Uiso 1 1 calc R . . H16B H 0.2554 0.0184 0.1716 0.136 Uiso 1 1 calc R . . H16C H 0.1582 -0.0069 0.1618 0.136 Uiso 1 1 calc R . . C17 C 0.2701(3) 0.2068(4) 0.1016(3) 0.133(2) Uani 1 1 d U . . H17A H 0.2575 0.2537 0.0683 0.200 Uiso 1 1 calc R . . H17B H 0.3145 0.1607 0.0981 0.200 Uiso 1 1 calc R . . H17C H 0.2889 0.2441 0.1388 0.200 Uiso 1 1 calc R . . C18 C 0.1521(4) 0.0485(5) 0.0341(2) 0.144(3) Uani 1 1 d U . . H18A H 0.1013 0.0088 0.0308 0.216 Uiso 1 1 calc R . . H18B H 0.2000 0.0035 0.0382 0.216 Uiso 1 1 calc R . . H18C H 0.1447 0.0894 -0.0016 0.216 Uiso 1 1 calc R . . C19 C -0.0541(4) 0.3498(5) 0.0567(3) 0.128(2) Uani 1 1 d U . . H19A H -0.0949 0.2967 0.0566 0.192 Uiso 1 1 calc R . . H19B H -0.0778 0.3968 0.0244 0.192 Uiso 1 1 calc R . . H19C H -0.0410 0.3855 0.0946 0.192 Uiso 1 1 calc R . . C20 C 0.1200(4) 0.4006(5) 0.0434(3) 0.147(3) Uani 1 1 d U . . H20A H 0.1781 0.3775 0.0585 0.221 Uiso 1 1 calc R . . H20B H 0.1101 0.4560 0.0680 0.221 Uiso 1 1 calc R . . H20C H 0.1101 0.4235 0.0025 0.221 Uiso 1 1 calc R . . C21 C 0.0150(5) 0.2388(5) -0.0311(2) 0.133(2) Uani 1 1 d U . . H21A H 0.0651 0.2124 -0.0402 0.200 Uiso 1 1 calc R . . H21B H -0.0100 0.2914 -0.0595 0.200 Uiso 1 1 calc R . . H21C H -0.0257 0.1846 -0.0335 0.200 Uiso 1 1 calc R . . C4 C 0.16600(16) 0.2753(2) 0.29003(13) 0.0432(6) Uani 1 1 d . . . C3 C 0.19353(19) 0.3180(2) 0.24444(16) 0.0543(7) Uani 1 1 d . . . H3 H 0.2423 0.3002 0.2331 0.065 Uiso 1 1 calc R . . C2 C 0.13329(19) 0.3948(2) 0.21786(15) 0.0582(8) Uani 1 1 d . . . H2 H 0.1347 0.4370 0.1856 0.070 Uiso 1 1 calc R . . C1 C 0.07247(17) 0.3946(2) 0.24912(14) 0.0495(7) Uani 1 1 d . . . C5 C 0.20682(17) 0.2031(2) 0.34031(14) 0.0481(7) Uani 1 1 d . . . C14 C 0.2415(2) 0.2630(3) 0.39934(16) 0.0687(9) Uani 1 1 d . . . H14A H 0.1973 0.3065 0.4058 0.103 Uiso 1 1 calc R . . H14B H 0.2894 0.3039 0.3967 0.103 Uiso 1 1 calc R . . H14C H 0.2595 0.2160 0.4325 0.103 Uiso 1 1 calc R . . C13 C 0.28170(19) 0.1436(3) 0.32860(18) 0.0685(9) Uani 1 1 d . . . H13A H 0.3061 0.0995 0.3623 0.103 Uiso 1 1 calc R . . H13B H 0.3245 0.1906 0.3235 0.103 Uiso 1 1 calc R . . H13C H 0.2615 0.1032 0.2926 0.103 Uiso 1 1 calc R . . C11 C 0.0000 0.4652(3) 0.2500 0.0621(12) Uani 1 2 d S . . C12 C -0.0262(3) 0.5335(3) 0.1936(2) 0.0911(14) Uani 1 1 d . . . H12A H -0.0433 0.4914 0.1581 0.137 Uiso 1 1 calc R . . H12B H 0.0214 0.5754 0.1916 0.137 Uiso 1 1 calc R . . H12C H -0.0733 0.5763 0.1958 0.137 Uiso 1 1 calc R . . N2 N 0.08988(13) 0.09064(16) 0.28718(10) 0.0388(4) Uani 1 1 d . . . C6 C 0.13586(16) 0.1303(2) 0.34240(12) 0.0439(6) Uani 1 1 d . . . C7 C 0.1107(2) 0.0862(2) 0.38871(14) 0.0568(7) Uani 1 1 d . . . H7 H 0.1296 0.1032 0.4295 0.068 Uiso 1 1 calc R . . C8 C 0.0501(2) 0.0094(2) 0.36218(14) 0.0542(7) Uani 1 1 d . . . H8 H 0.0215 -0.0338 0.3822 0.065 Uiso 1 1 calc R . . C9 C 0.04205(16) 0.01133(19) 0.30114(12) 0.0413(5) Uani 1 1 d . . . C10 C 0.0000 -0.0588(3) 0.2500 0.0446(8) Uani 1 2 d S . . C15 C 0.0680(2) -0.1280(2) 0.23521(17) 0.0620(8) Uani 1 1 d . . . H15A H 0.1138 -0.0867 0.2292 0.093 Uiso 1 1 calc R . . H15B H 0.0426 -0.1661 0.1991 0.093 Uiso 1 1 calc R . . H15C H 0.0902 -0.1744 0.2681 0.093 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 Sm1 0.03615(8) 0.03711(8) 0.03813(8) 0.00255(5) 0.01105(5) -0.00128(5) Si1 0.0639(5) 0.0726(6) 0.0460(4) 0.0076(4) 0.0242(4) 0.0114(4) Si2 0.0771(6) 0.0731(6) 0.0569(5) 0.0242(5) 0.0256(5) 0.0097(5) N3 0.0552(14) 0.0530(14) 0.0431(13) 0.0088(10) 0.0184(11) -0.0004(11) N1 0.0373(11) 0.0358(11) 0.0512(13) -0.0026(9) 0.0066(9) -0.0011(9) C16 0.101(3) 0.098(3) 0.084(3) 0.034(2) 0.043(2) 0.039(2) C17 0.079(3) 0.153(5) 0.185(6) 0.059(4) 0.066(4) 0.009(3) C18 0.176(5) 0.154(5) 0.085(3) -0.040(3) 0.008(3) 0.073(4) C19 0.136(4) 0.134(4) 0.129(4) 0.070(4) 0.063(4) 0.073(4) C20 0.159(5) 0.119(4) 0.166(5) 0.078(4) 0.048(4) -0.019(4) C21 0.166(5) 0.150(5) 0.068(3) 0.013(3) 0.005(3) 0.038(4) C4 0.0332(12) 0.0403(13) 0.0527(15) -0.0052(11) 0.0061(11) -0.0051(10) C3 0.0402(14) 0.0533(17) 0.070(2) -0.0033(14) 0.0153(13) -0.0125(12) C2 0.0533(16) 0.0506(17) 0.0671(19) 0.0093(15) 0.0108(14) -0.0178(14) C1 0.0457(14) 0.0331(13) 0.0633(17) 0.0017(12) 0.0046(13) -0.0072(11) C5 0.0359(13) 0.0466(15) 0.0545(16) -0.0024(12) 0.0001(11) 0.0008(11) C14 0.0561(18) 0.072(2) 0.062(2) -0.0097(17) -0.0092(16) -0.0071(17) C13 0.0403(15) 0.068(2) 0.093(3) 0.0005(19) 0.0108(16) 0.0108(14) C11 0.051(2) 0.031(2) 0.091(3) 0.000 -0.001(2) 0.000 C12 0.073(2) 0.049(2) 0.136(4) 0.038(2) 0.003(2) -0.0029(17) N2 0.0356(10) 0.0362(11) 0.0444(11) 0.0023(9) 0.0110(9) 0.0023(8) C6 0.0399(12) 0.0431(14) 0.0439(14) 0.0029(11) 0.0034(11) 0.0046(11) C7 0.0629(18) 0.0598(19) 0.0419(15) 0.0075(13) 0.0048(13) 0.0034(15) C8 0.0606(17) 0.0505(16) 0.0526(16) 0.0141(13) 0.0176(14) 0.0018(14) C9 0.0398(12) 0.0344(12) 0.0501(14) 0.0056(11) 0.0129(11) 0.0038(10) C10 0.0451(19) 0.0327(18) 0.058(2) 0.000 0.0169(17) 0.000 C15 0.0598(18) 0.0422(16) 0.088(2) -0.0003(15) 0.0268(17) 0.0109(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N3 2.286(2) . ? Sm1 N1 2.666(2) 2 ? Sm1 N2 2.671(2) . ? Sm1 N2 2.725(2) 2 ? Sm1 N1 2.748(2) . ? Sm1 C6 2.860(3) 2 ? Sm1 C4 2.861(3) . ? Sm1 C9 2.863(3) 2 ? Sm1 C1 2.865(3) . ? Sm1 C3 2.941(3) . ? Sm1 C2 2.941(3) . ? Sm1 C7 2.967(3) 2 ? Si1 N3 1.712(3) . ? Si1 C18 1.844(5) . ? Si1 C16 1.845(4) . ? Si1 C17 1.868(5) . ? Si2 N3 1.714(2) . ? Si2 C21 1.847(6) . ? Si2 C19 1.855(5) . ? Si2 C20 1.877(5) . ? N1 C4 1.384(3) . ? N1 C1 1.387(4) . ? N1 Sm1 2.666(2) 2 ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C4 C3 1.369(4) . ? C4 C5 1.500(4) . ? C3 C2 1.418(4) . ? C3 H3 0.9300 . ? C2 C1 1.374(4) . ? C2 H2 0.9300 . ? C1 C11 1.501(4) . ? C5 C6 1.506(4) . ? C5 C13 1.530(4) . ? C5 C14 1.535(4) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C11 C1 1.501(4) 2 ? C11 C12 1.536(4) . ? C11 C12 1.536(4) 2 ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? N2 C6 1.385(3) . ? N2 C9 1.386(3) . ? N2 Sm1 2.725(2) 2 ? C6 C7 1.370(4) . ? C6 Sm1 2.860(3) 2 ? C7 C8 1.422(4) . ? C7 Sm1 2.967(3) 2 ? C7 H7 0.9300 . ? C8 C9 1.375(4) . ? C8 Sm1 2.968(3) 2 ? C8 H8 0.9300 . ? C9 C10 1.500(3) . ? C9 Sm1 2.863(3) 2 ? C10 C9 1.500(3) 2 ? C10 C15 1.538(4) . ? C10 C15 1.538(4) 2 ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? 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 N3 Sm1 N1 127.49(8) . 2 ? N3 Sm1 N2 129.49(8) . . ? N1 Sm1 N2 102.99(7) 2 . ? N3 Sm1 N2 131.63(8) . 2 ? N1 Sm1 N2 66.42(7) 2 2 ? N2 Sm1 N2 66.27(8) . 2 ? N3 Sm1 N1 128.90(8) . . ? N1 Sm1 N1 66.36(8) 2 . ? N2 Sm1 N1 66.02(7) . . ? N2 Sm1 N1 99.46(7) 2 . ? N3 Sm1 C6 111.36(9) . 2 ? N1 Sm1 C6 58.87(7) 2 2 ? N2 Sm1 C6 94.76(7) . 2 ? N2 Sm1 C6 28.60(7) 2 2 ? N1 Sm1 C6 115.24(7) . 2 ? N3 Sm1 C4 109.74(9) . . ? N1 Sm1 C4 94.73(7) 2 . ? N2 Sm1 C4 58.47(7) . . ? N2 Sm1 C4 115.01(7) 2 . ? N1 Sm1 C4 28.48(7) . . ? C6 Sm1 C4 138.89(8) 2 . ? N3 Sm1 C9 112.14(8) . 2 ? N1 Sm1 C9 94.92(7) 2 2 ? N2 Sm1 C9 58.76(7) . 2 ? N2 Sm1 C9 28.60(7) 2 2 ? N1 Sm1 C9 115.07(7) . 2 ? C6 Sm1 C9 45.26(7) 2 2 ? C4 Sm1 C9 117.08(8) . 2 ? N3 Sm1 C1 109.02(9) . . ? N1 Sm1 C1 58.68(7) 2 . ? N2 Sm1 C1 94.44(7) . . ? N2 Sm1 C1 115.09(8) 2 . ? N1 Sm1 C1 28.51(7) . . ? C6 Sm1 C1 117.36(8) 2 . ? C4 Sm1 C1 45.19(8) . . ? C9 Sm1 C1 138.84(8) 2 . ? N3 Sm1 C3 84.18(9) . . ? N1 Sm1 C3 103.91(8) 2 . ? N2 Sm1 C3 81.92(8) . . ? N2 Sm1 C3 142.22(8) 2 . ? N1 Sm1 C3 46.79(8) . . ? C6 Sm1 C3 161.44(9) 2 . ? C4 Sm1 C3 27.25(9) . . ? C9 Sm1 C3 139.44(8) 2 . ? C1 Sm1 C3 45.30(9) . . ? N3 Sm1 C2 83.68(9) . . ? N1 Sm1 C2 82.14(8) 2 . ? N2 Sm1 C2 103.70(8) . . ? N2 Sm1 C2 142.39(8) 2 . ? N1 Sm1 C2 46.86(8) . . ? C6 Sm1 C2 139.83(8) 2 . ? C4 Sm1 C2 45.30(8) . . ? C9 Sm1 C2 161.26(9) 2 . ? C1 Sm1 C2 27.34(9) . . ? C3 Sm1 C2 27.90(9) . . ? N3 Sm1 C7 86.43(9) . 2 ? N1 Sm1 C7 82.21(8) 2 2 ? N2 Sm1 C7 103.87(8) . 2 ? N2 Sm1 C7 46.74(8) 2 2 ? N1 Sm1 C7 142.32(8) . 2 ? C6 Sm1 C7 27.13(8) 2 2 ? C4 Sm1 C7 161.10(9) . 2 ? C9 Sm1 C7 45.20(8) 2 2 ? C1 Sm1 C7 139.78(8) . 2 ? C3 Sm1 C7 170.60(9) . 2 ? C2 Sm1 C7 150.70(9) . 2 ? N3 Si1 C18 114.7(2) . . ? N3 Si1 C16 109.58(16) . . ? C18 Si1 C16 106.1(3) . . ? N3 Si1 C17 113.3(2) . . ? C18 Si1 C17 105.6(3) . . ? C16 Si1 C17 107.0(3) . . ? N3 Si2 C21 116.0(2) . . ? N3 Si2 C19 109.37(18) . . ? C21 Si2 C19 105.7(3) . . ? N3 Si2 C20 113.0(2) . . ? C21 Si2 C20 104.9(3) . . ? C19 Si2 C20 107.2(3) . . ? Si1 N3 Si2 119.67(15) . . ? Si1 N3 Sm1 119.53(12) . . ? Si2 N3 Sm1 120.64(13) . . ? C4 N1 C1 105.1(2) . . ? C4 N1 Sm1 122.52(17) . 2 ? C1 N1 Sm1 122.84(17) . 2 ? C4 N1 Sm1 80.31(15) . . ? C1 N1 Sm1 80.43(16) . . ? Sm1 N1 Sm1 78.61(6) 2 . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si1 C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C3 C4 N1 110.7(3) . . ? C3 C4 C5 132.9(3) . . ? N1 C4 C5 116.1(3) . . ? C3 C4 Sm1 79.60(17) . . ? N1 C4 Sm1 71.21(14) . . ? C5 C4 Sm1 119.91(16) . . ? C4 C3 C2 106.7(3) . . ? C4 C3 Sm1 73.15(15) . . ? C2 C3 Sm1 76.05(16) . . ? C4 C3 H3 126.7 . . ? C2 C3 H3 126.7 . . ? Sm1 C3 H3 116.4 . . ? C1 C2 C3 106.5(3) . . ? C1 C2 Sm1 73.27(16) . . ? C3 C2 Sm1 76.05(16) . . ? C1 C2 H2 126.8 . . ? C3 C2 H2 126.8 . . ? Sm1 C2 H2 116.2 . . ? C2 C1 N1 110.5(3) . . ? C2 C1 C11 133.4(3) . . ? N1 C1 C11 115.9(3) . . ? C2 C1 Sm1 79.39(18) . . ? N1 C1 Sm1 71.05(14) . . ? C11 C1 Sm1 119.55(17) . . ? C4 C5 C6 104.1(2) . . ? C4 C5 C13 112.8(3) . . ? C6 C5 C13 109.7(2) . . ? C4 C5 C14 109.7(2) . . ? C6 C5 C14 113.0(3) . . ? C13 C5 C14 107.5(3) . . ? C5 C14 H14A 109.5 . . ? C5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C5 C13 H13A 109.5 . . ? C5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C1 C11 C1 104.1(3) 2 . ? C1 C11 C12 109.48(18) 2 . ? C1 C11 C12 112.4(2) . . ? C1 C11 C12 112.4(2) 2 2 ? C1 C11 C12 109.48(18) . 2 ? C12 C11 C12 108.9(4) . 2 ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 N2 C9 105.2(2) . . ? C6 N2 Sm1 123.41(16) . . ? C9 N2 Sm1 122.96(16) . . ? C6 N2 Sm1 81.11(14) . 2 ? C9 N2 Sm1 81.24(14) . 2 ? Sm1 N2 Sm1 78.94(5) . 2 ? C7 C6 N2 110.8(2) . . ? C7 C6 C5 133.3(3) . . ? N2 C6 C5 115.5(2) . . ? C7 C6 Sm1 80.79(17) . 2 ? N2 C6 Sm1 70.30(13) . 2 ? C5 C6 Sm1 119.44(17) . 2 ? C6 C7 C8 106.5(3) . . ? C6 C7 Sm1 72.08(16) . 2 ? C8 C7 Sm1 76.17(17) . 2 ? C6 C7 H7 126.8 . . ? C8 C7 H7 126.8 . . ? Sm1 C7 H7 117.2 2 . ? C9 C8 C7 106.5(3) . . ? C9 C8 Sm1 72.15(16) . 2 ? C7 C8 Sm1 76.10(17) . 2 ? C9 C8 H8 126.7 . . ? C7 C8 H8 126.7 . . ? Sm1 C8 H8 117.2 2 . ? C8 C9 N2 110.5(2) . . ? C8 C9 C10 133.2(2) . . ? N2 C9 C10 116.0(2) . . ? C8 C9 Sm1 80.64(17) . 2 ? N2 C9 Sm1 70.17(13) . 2 ? C10 C9 Sm1 119.50(16) . 2 ? C9 C10 C9 104.6(3) . 2 ? C9 C10 C15 109.54(16) . . ? C9 C10 C15 112.67(17) 2 . ? C9 C10 C15 112.67(17) . 2 ? C9 C10 C15 109.54(16) 2 2 ? C15 C10 C15 107.9(3) . 2 ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C18 Si1 N3 Si2 -59.1(3) . . . . ? C16 Si1 N3 Si2 -178.3(2) . . . . ? C17 Si1 N3 Si2 62.2(3) . . . . ? C18 Si1 N3 Sm1 125.5(3) . . . . ? C16 Si1 N3 Sm1 6.3(2) . . . . ? C17 Si1 N3 Sm1 -113.1(3) . . . . ? C21 Si2 N3 Si1 53.1(3) . . . . ? C19 Si2 N3 Si1 172.5(3) . . . . ? C20 Si2 N3 Si1 -68.2(3) . . . . ? C21 Si2 N3 Sm1 -131.6(3) . . . . ? C19 Si2 N3 Sm1 -12.2(3) . . . . ? C20 Si2 N3 Sm1 107.1(3) . . . . ? N1 Sm1 N3 Si1 176.55(11) 2 . . . ? N2 Sm1 N3 Si1 -1.04(19) . . . . ? N2 Sm1 N3 Si1 -93.03(16) 2 . . . ? N1 Sm1 N3 Si1 88.30(15) . . . . ? C6 Sm1 N3 Si1 -117.01(14) 2 . . . ? C4 Sm1 N3 Si1 63.86(16) . . . . ? C9 Sm1 N3 Si1 -68.07(16) 2 . . . ? C1 Sm1 N3 Si1 111.93(14) . . . . ? C3 Sm1 N3 Si1 73.47(15) . . . . ? C2 Sm1 N3 Si1 101.53(15) . . . . ? C7 Sm1 N3 Si1 -106.10(15) 2 . . . ? N1 Sm1 N3 Si2 1.2(2) 2 . . . ? N2 Sm1 N3 Si2 -176.36(11) . . . . ? N2 Sm1 N3 Si2 91.65(16) 2 . . . ? N1 Sm1 N3 Si2 -87.03(17) . . . . ? C6 Sm1 N3 Si2 67.67(16) 2 . . . ? C4 Sm1 N3 Si2 -111.46(15) . . . . ? C9 Sm1 N3 Si2 116.61(14) 2 . . . ? C1 Sm1 N3 Si2 -63.40(16) . . . . ? C3 Sm1 N3 Si2 -101.85(16) . . . . ? C2 Sm1 N3 Si2 -73.80(15) . . . . ? C7 Sm1 N3 Si2 78.57(15) 2 . . . ? N3 Sm1 N1 C4 -54.73(18) . . . . ? N1 Sm1 N1 C4 -174.76(17) 2 . . . ? N2 Sm1 N1 C4 67.64(15) . . . . ? N2 Sm1 N1 C4 126.27(16) 2 . . . ? C6 Sm1 N1 C4 151.38(15) 2 . . . ? C9 Sm1 N1 C4 101.06(16) 2 . . . ? C1 Sm1 N1 C4 -107.3(2) . . . . ? C3 Sm1 N1 C4 -34.29(16) . . . . ? C2 Sm1 N1 C4 -72.89(17) . . . . ? C7 Sm1 N1 C4 149.22(17) 2 . . . ? N3 Sm1 N1 C1 52.55(18) . . . . ? N1 Sm1 N1 C1 -67.48(14) 2 . . . ? N2 Sm1 N1 C1 174.93(17) . . . . ? N2 Sm1 N1 C1 -126.45(15) 2 . . . ? C6 Sm1 N1 C1 -101.34(16) 2 . . . ? C4 Sm1 N1 C1 107.3(2) . . . . ? C9 Sm1 N1 C1 -151.65(15) 2 . . . ? C3 Sm1 N1 C1 72.99(17) . . . . ? C2 Sm1 N1 C1 34.39(16) . . . . ? C7 Sm1 N1 C1 -103.50(19) 2 . . . ? N3 Sm1 N1 Sm1 179.06(8) . . . 2 ? N1 Sm1 N1 Sm1 59.03(8) 2 . . 2 ? N2 Sm1 N1 Sm1 -58.57(6) . . . 2 ? N2 Sm1 N1 Sm1 0.06(6) 2 . . 2 ? C6 Sm1 N1 Sm1 25.16(8) 2 . . 2 ? C4 Sm1 N1 Sm1 -126.21(17) . . . 2 ? C9 Sm1 N1 Sm1 -25.15(8) 2 . . 2 ? C1 Sm1 N1 Sm1 126.50(17) . . . 2 ? C3 Sm1 N1 Sm1 -160.50(12) . . . 2 ? C2 Sm1 N1 Sm1 160.89(12) . . . 2 ? C7 Sm1 N1 Sm1 23.01(14) 2 . . 2 ? C1 N1 C4 C3 -6.7(3) . . . . ? Sm1 N1 C4 C3 140.3(2) 2 . . . ? Sm1 N1 C4 C3 70.6(2) . . . . ? C1 N1 C4 C5 167.9(2) . . . . ? Sm1 N1 C4 C5 -45.1(3) 2 . . . ? Sm1 N1 C4 C5 -114.8(2) . . . . ? C1 N1 C4 Sm1 -77.25(17) . . . . ? Sm1 N1 C4 Sm1 69.73(14) 2 . . . ? N3 Sm1 C4 C3 21.3(2) . . . . ? N1 Sm1 C4 C3 -111.46(18) 2 . . . ? N2 Sm1 C4 C3 146.2(2) . . . . ? N2 Sm1 C4 C3 -177.62(17) 2 . . . ? N1 Sm1 C4 C3 -116.3(2) . . . . ? C6 Sm1 C4 C3 -157.50(17) 2 . . . ? C9 Sm1 C4 C3 150.55(17) 2 . . . ? C1 Sm1 C4 C3 -76.3(2) . . . . ? C2 Sm1 C4 C3 -37.43(18) . . . . ? C7 Sm1 C4 C3 168.8(2) 2 . . . ? N3 Sm1 C4 N1 137.54(15) . . . . ? N1 Sm1 C4 N1 4.82(16) 2 . . . ? N2 Sm1 C4 N1 -97.53(17) . . . . ? N2 Sm1 C4 N1 -61.34(17) 2 . . . ? C6 Sm1 C4 N1 -41.2(2) 2 . . . ? C9 Sm1 C4 N1 -93.17(16) 2 . . . ? C1 Sm1 C4 N1 39.97(15) . . . . ? C3 Sm1 C4 N1 116.3(2) . . . . ? C2 Sm1 C4 N1 78.85(17) . . . . ? C7 Sm1 C4 N1 -74.9(3) 2 . . . ? N3 Sm1 C4 C5 -112.6(2) . . . . ? N1 Sm1 C4 C5 114.7(2) 2 . . . ? N2 Sm1 C4 C5 12.34(19) . . . . ? N2 Sm1 C4 C5 48.5(2) 2 . . . ? N1 Sm1 C4 C5 109.9(3) . . . . ? C6 Sm1 C4 C5 68.6(2) 2 . . . ? C9 Sm1 C4 C5 16.7(2) 2 . . . ? C1 Sm1 C4 C5 149.8(3) . . . . ? C3 Sm1 C4 C5 -133.8(3) . . . . ? C2 Sm1 C4 C5 -171.3(3) . . . . ? C7 Sm1 C4 C5 34.9(4) 2 . . . ? N1 C4 C3 C2 4.1(3) . . . . ? C5 C4 C3 C2 -169.3(3) . . . . ? Sm1 C4 C3 C2 69.3(2) . . . . ? N1 C4 C3 Sm1 -65.19(18) . . . . ? C5 C4 C3 Sm1 121.4(3) . . . . ? N3 Sm1 C3 C4 -159.93(19) . . . . ? N1 Sm1 C3 C4 72.84(18) 2 . . . ? N2 Sm1 C3 C4 -28.62(17) . . . . ? N2 Sm1 C3 C4 3.5(2) 2 . . . ? N1 Sm1 C3 C4 35.92(16) . . . . ? C6 Sm1 C3 C4 52.2(4) 2 . . . ? C9 Sm1 C3 C4 -42.3(2) 2 . . . ? C1 Sm1 C3 C4 75.9(2) . . . . ? C2 Sm1 C3 C4 112.6(3) . . . . ? C7 Sm1 C3 C4 -157.3(5) 2 . . . ? N3 Sm1 C3 C2 87.5(2) . . . . ? N1 Sm1 C3 C2 -39.8(2) 2 . . . ? N2 Sm1 C3 C2 -141.2(2) . . . . ? N2 Sm1 C3 C2 -109.1(2) 2 . . . ? N1 Sm1 C3 C2 -76.7(2) . . . . ? C6 Sm1 C3 C2 -60.4(4) 2 . . . ? C4 Sm1 C3 C2 -112.6(3) . . . . ? C9 Sm1 C3 C2 -154.91(18) 2 . . . ? C1 Sm1 C3 C2 -36.71(19) . . . . ? C7 Sm1 C3 C2 90.1(6) 2 . . . ? C4 C3 C2 C1 0.2(3) . . . . ? Sm1 C3 C2 C1 67.5(2) . . . . ? C4 C3 C2 Sm1 -67.3(2) . . . . ? N3 Sm1 C2 C1 158.18(19) . . . . ? N1 Sm1 C2 C1 28.88(18) 2 . . . ? N2 Sm1 C2 C1 -72.65(18) . . . . ? N2 Sm1 C2 C1 -3.9(2) 2 . . . ? N1 Sm1 C2 C1 -35.94(16) . . . . ? C6 Sm1 C2 C1 42.3(2) 2 . . . ? C4 Sm1 C2 C1 -75.82(19) . . . . ? C9 Sm1 C2 C1 -53.2(3) 2 . . . ? C3 Sm1 C2 C1 -112.3(3) . . . . ? C7 Sm1 C2 C1 87.2(3) 2 . . . ? N3 Sm1 C2 C3 -89.5(2) . . . . ? N1 Sm1 C2 C3 141.2(2) 2 . . . ? N2 Sm1 C2 C3 39.7(2) . . . . ? N2 Sm1 C2 C3 108.4(2) 2 . . . ? N1 Sm1 C2 C3 76.4(2) . . . . ? C6 Sm1 C2 C3 154.59(18) 2 . . . ? C4 Sm1 C2 C3 36.49(19) . . . . ? C9 Sm1 C2 C3 59.1(4) 2 . . . ? C1 Sm1 C2 C3 112.3(3) . . . . ? C7 Sm1 C2 C3 -160.5(2) 2 . . . ? C3 C2 C1 N1 -4.4(3) . . . . ? Sm1 C2 C1 N1 64.99(19) . . . . ? C3 C2 C1 C11 169.7(3) . . . . ? Sm1 C2 C1 C11 -120.9(3) . . . . ? C3 C2 C1 Sm1 -69.4(2) . . . . ? C4 N1 C1 C2 6.8(3) . . . . ? Sm1 N1 C1 C2 -140.0(2) 2 . . . ? Sm1 N1 C1 C2 -70.3(2) . . . . ? C4 N1 C1 C11 -168.5(2) . . . . ? Sm1 N1 C1 C11 44.7(3) 2 . . . ? Sm1 N1 C1 C11 114.4(2) . . . . ? C4 N1 C1 Sm1 77.15(17) . . . . ? Sm1 N1 C1 Sm1 -69.69(15) 2 . . . ? N3 Sm1 C1 C2 -23.0(2) . . . . ? N1 Sm1 C1 C2 -145.9(2) 2 . . . ? N2 Sm1 C1 C2 111.55(18) . . . . ? N2 Sm1 C1 C2 177.38(17) 2 . . . ? N1 Sm1 C1 C2 116.2(2) . . . . ? C6 Sm1 C1 C2 -150.76(17) 2 . . . ? C4 Sm1 C1 C2 76.27(19) . . . . ? C9 Sm1 C1 C2 156.99(17) 2 . . . ? C3 Sm1 C1 C2 37.52(18) . . . . ? C7 Sm1 C1 C2 -130.80(19) 2 . . . ? N3 Sm1 C1 N1 -139.19(15) . . . . ? N1 Sm1 C1 N1 97.87(16) 2 . . . ? N2 Sm1 C1 N1 -4.65(16) . . . . ? N2 Sm1 C1 N1 61.19(16) 2 . . . ? C6 Sm1 C1 N1 93.05(16) 2 . . . ? C4 Sm1 C1 N1 -39.93(15) . . . . ? C9 Sm1 C1 N1 40.8(2) 2 . . . ? C3 Sm1 C1 N1 -78.68(17) . . . . ? C2 Sm1 C1 N1 -116.2(2) . . . . ? C7 Sm1 C1 N1 113.01(17) 2 . . . ? N3 Sm1 C1 C11 111.2(2) . . . . ? N1 Sm1 C1 C11 -11.77(17) 2 . . . ? N2 Sm1 C1 C11 -114.29(19) . . . . ? N2 Sm1 C1 C11 -48.5(2) 2 . . . ? N1 Sm1 C1 C11 -109.6(3) . . . . ? C6 Sm1 C1 C11 -16.6(2) 2 . . . ? C4 Sm1 C1 C11 -149.6(3) . . . . ? C9 Sm1 C1 C11 -68.8(2) 2 . . . ? C3 Sm1 C1 C11 171.7(3) . . . . ? C2 Sm1 C1 C11 134.2(3) . . . . ? C7 Sm1 C1 C11 3.4(3) 2 . . . ? C3 C4 C5 C6 -138.4(3) . . . . ? N1 C4 C5 C6 48.4(3) . . . . ? Sm1 C4 C5 C6 -34.0(3) . . . . ? C3 C4 C5 C13 -19.5(4) . . . . ? N1 C4 C5 C13 167.4(2) . . . . ? Sm1 C4 C5 C13 85.0(3) . . . . ? C3 C4 C5 C14 100.3(4) . . . . ? N1 C4 C5 C14 -72.8(3) . . . . ? Sm1 C4 C5 C14 -155.2(2) . . . . ? C2 C1 C11 C1 137.7(4) . . . 2 ? N1 C1 C11 C1 -48.39(17) . . . 2 ? Sm1 C1 C11 C1 33.58(8) . . . 2 ? C2 C1 C11 C12 19.3(4) . . . . ? N1 C1 C11 C12 -166.8(3) . . . . ? Sm1 C1 C11 C12 -84.8(3) . . . . ? C2 C1 C11 C12 -101.9(4) . . . 2 ? N1 C1 C11 C12 72.0(3) . . . 2 ? Sm1 C1 C11 C12 154.0(3) . . . 2 ? N3 Sm1 N2 C6 106.6(2) . . . . ? N1 Sm1 N2 C6 -71.4(2) 2 . . . ? N2 Sm1 N2 C6 -128.1(2) 2 . . . ? N1 Sm1 N2 C6 -15.00(19) . . . . ? C6 Sm1 N2 C6 -130.54(18) 2 . . . ? C4 Sm1 N2 C6 16.16(19) . . . . ? C9 Sm1 N2 C6 -159.3(2) 2 . . . ? C1 Sm1 N2 C6 -12.6(2) . . . . ? C3 Sm1 N2 C6 31.1(2) . . . . ? C2 Sm1 N2 C6 13.5(2) . . . . ? C7 Sm1 N2 C6 -156.47(19) 2 . . . ? N3 Sm1 N2 C9 -110.1(2) . . . . ? N1 Sm1 N2 C9 71.90(19) 2 . . . ? N2 Sm1 N2 C9 15.25(18) 2 . . . ? N1 Sm1 N2 C9 128.3(2) . . . . ? C6 Sm1 N2 C9 12.8(2) 2 . . . ? C4 Sm1 N2 C9 159.5(2) . . . . ? C9 Sm1 N2 C9 -16.0(2) 2 . . . ? C1 Sm1 N2 C9 130.75(19) . . . . ? C3 Sm1 N2 C9 174.4(2) . . . . ? C2 Sm1 N2 C9 156.84(19) . . . . ? C7 Sm1 N2 C9 -13.2(2) 2 . . . ? N3 Sm1 N2 Sm1 178.10(8) . . . 2 ? N1 Sm1 N2 Sm1 0.06(6) 2 . . 2 ? N2 Sm1 N2 Sm1 -56.59(7) 2 . . 2 ? N1 Sm1 N2 Sm1 56.49(6) . . . 2 ? C6 Sm1 N2 Sm1 -59.06(7) 2 . . 2 ? C4 Sm1 N2 Sm1 87.65(8) . . . 2 ? C9 Sm1 N2 Sm1 -87.82(8) 2 . . 2 ? C1 Sm1 N2 Sm1 58.91(7) . . . 2 ? C3 Sm1 N2 Sm1 102.56(8) . . . 2 ? C2 Sm1 N2 Sm1 85.00(8) . . . 2 ? C7 Sm1 N2 Sm1 -84.99(8) 2 . . 2 ? C9 N2 C6 C7 -6.9(3) . . . . ? Sm1 N2 C6 C7 141.8(2) . . . . ? Sm1 N2 C6 C7 71.5(2) 2 . . . ? C9 N2 C6 C5 167.6(2) . . . . ? Sm1 N2 C6 C5 -43.7(3) . . . . ? Sm1 N2 C6 C5 -114.0(2) 2 . . . ? C9 N2 C6 Sm1 -78.33(16) . . . 2 ? Sm1 N2 C6 Sm1 70.38(13) . . . 2 ? C4 C5 C6 C7 -139.4(3) . . . . ? C13 C5 C6 C7 99.6(4) . . . . ? C14 C5 C6 C7 -20.4(4) . . . . ? C4 C5 C6 N2 47.7(3) . . . . ? C13 C5 C6 N2 -73.3(3) . . . . ? C14 C5 C6 N2 166.7(2) . . . . ? C4 C5 C6 Sm1 -33.1(3) . . . 2 ? C13 C5 C6 Sm1 -154.1(2) . . . 2 ? C14 C5 C6 Sm1 85.9(3) . . . 2 ? N2 C6 C7 C8 4.3(3) . . . . ? C5 C6 C7 C8 -168.8(3) . . . . ? Sm1 C6 C7 C8 69.0(2) 2 . . . ? N2 C6 C7 Sm1 -64.72(18) . . . 2 ? C5 C6 C7 Sm1 122.1(3) . . . 2 ? C6 C7 C8 C9 0.0(3) . . . . ? Sm1 C7 C8 C9 66.2(2) 2 . . . ? C6 C7 C8 Sm1 -66.2(2) . . . 2 ? C7 C8 C9 N2 -4.4(3) . . . . ? Sm1 C8 C9 N2 64.61(17) 2 . . . ? C7 C8 C9 C10 169.0(3) . . . . ? Sm1 C8 C9 C10 -122.0(3) 2 . . . ? C7 C8 C9 Sm1 -69.0(2) . . . 2 ? C6 N2 C9 C8 6.9(3) . . . . ? Sm1 N2 C9 C8 -142.02(19) . . . . ? Sm1 N2 C9 C8 -71.4(2) 2 . . . ? C6 N2 C9 C10 -167.8(2) . . . . ? Sm1 N2 C9 C10 43.3(3) . . . . ? Sm1 N2 C9 C10 113.98(19) 2 . . . ? C6 N2 C9 Sm1 78.23(16) . . . 2 ? Sm1 N2 C9 Sm1 -70.65(13) . . . 2 ? C8 C9 C10 C9 139.3(3) . . . 2 ? N2 C9 C10 C9 -47.53(16) . . . 2 ? Sm1 C9 C10 C9 33.40(7) 2 . . 2 ? C8 C9 C10 C15 -99.7(3) . . . . ? N2 C9 C10 C15 73.5(3) . . . . ? Sm1 C9 C10 C15 154.39(19) 2 . . . ? C8 C9 C10 C15 20.5(4) . . . 2 ? N2 C9 C10 C15 -166.4(2) . . . 2 ? Sm1 C9 C10 C15 -85.5(3) 2 . . 2 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.448 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.106 # Attachment '4905_web_deposit_cif_file_2_ShuangliuZhou_1301667625.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 819829' #TrackingRef '4905_web_deposit_cif_file_2_ShuangliuZhou_1301667625.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H68 Dy2 N6 Si4' _chemical_formula_weight 1070.36 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' Dy Dy -0.1892 4.4098 '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 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 16.314(3) _cell_length_b 13.062(3) _cell_length_c 22.806(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.693(2) _cell_angle_gamma 90.00 _cell_volume 4678.4(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 3.305 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6369 _exptl_absorpt_correction_T_max 0.6925 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18762 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.52 _reflns_number_total 5347 _reflns_number_gt 4071 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+31.6616P] 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 5347 _refine_ls_number_parameters 246 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.132 _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 Dy Dy 1.036739(17) 0.20558(2) 0.188583(12) 0.04216(12) Uani 1 1 d . . . Si1 Si 1.17091(15) 0.1351(2) 0.10312(9) 0.0659(6) Uani 1 1 d U . . Si2 Si 1.04507(19) 0.2922(2) 0.04705(11) 0.0757(7) Uani 1 1 d U . . N3 N 1.0856(4) 0.2093(4) 0.1065(2) 0.0531(14) Uani 1 1 d . . . N2 N 0.9142(3) 0.3170(4) 0.2092(3) 0.0457(12) Uani 1 1 d . . . N1 N 0.9134(3) 0.0949(4) 0.2120(2) 0.0437(11) Uani 1 1 d . . . C16 C 1.1550(10) 0.0536(11) 0.0358(6) 0.141(5) Uani 1 1 d U . . H16A H 1.1091 0.0068 0.0342 0.211 Uiso 1 1 calc R . . H16B H 1.2061 0.0157 0.0379 0.211 Uiso 1 1 calc R . . H16C H 1.1413 0.0954 -0.0002 0.211 Uiso 1 1 calc R . . C17 C 1.2687(10) 0.2093(11) 0.1046(8) 0.138(5) Uani 1 1 d U . . H17A H 1.2550 0.2628 0.0747 0.207 Uiso 1 1 calc R . . H17B H 1.3104 0.1646 0.0956 0.207 Uiso 1 1 calc R . . H17C H 1.2912 0.2388 0.1442 0.207 Uiso 1 1 calc R . . C18 C 1.1998(8) 0.0491(9) 0.1694(5) 0.102(3) Uani 1 1 d U . . H18A H 1.1786 0.0766 0.2015 0.153 Uiso 1 1 calc R . . H18B H 1.2607 0.0432 0.1833 0.153 Uiso 1 1 calc R . . H18C H 1.1754 -0.0172 0.1580 0.153 Uiso 1 1 calc R . . C21 C 0.9511(10) 0.3583(12) 0.0577(7) 0.136(5) Uani 1 1 d U . . H21A H 0.9054 0.3102 0.0535 0.204 Uiso 1 1 calc R . . H21B H 0.9342 0.4111 0.0276 0.204 Uiso 1 1 calc R . . H21C H 0.9645 0.3882 0.0976 0.204 Uiso 1 1 calc R . . C19 C 1.0135(12) 0.2346(13) -0.0294(7) 0.152(6) Uani 1 1 d U . . H19A H 1.0617 0.2010 -0.0374 0.228 Uiso 1 1 calc R . . H19B H 0.9934 0.2872 -0.0592 0.228 Uiso 1 1 calc R . . H19C H 0.9690 0.1855 -0.0315 0.228 Uiso 1 1 calc R . . C20 C 1.1199(10) 0.3946(11) 0.0400(7) 0.154(6) Uani 1 1 d U . . H20A H 1.1250 0.4432 0.0724 0.230 Uiso 1 1 calc R . . H20B H 1.0990 0.4285 0.0015 0.230 Uiso 1 1 calc R . . H20C H 1.1747 0.3653 0.0425 0.230 Uiso 1 1 calc R . . C9 C 0.9282(4) 0.3955(5) 0.2509(3) 0.0547(16) Uani 1 1 d . . . C8 C 0.8666(5) 0.3966(6) 0.2814(4) 0.066(2) Uani 1 1 d . . . H8 H 0.8643 0.4397 0.3133 0.079 Uiso 1 1 calc R . . C7 C 0.8072(5) 0.3197(6) 0.2550(4) 0.0622(19) Uani 1 1 d . . . H7 H 0.7583 0.3020 0.2662 0.075 Uiso 1 1 calc R . . C6 C 0.8362(4) 0.2764(5) 0.2098(3) 0.0520(16) Uani 1 1 d . . . C10 C 1.0000 0.4665(8) 0.2500 0.066(3) Uani 1 2 d S . . C15 C 0.9729(7) 0.5354(7) 0.1930(5) 0.106(4) Uani 1 1 d . . . H15A H 0.9523 0.4935 0.1575 0.159 Uiso 1 1 calc R . . H15B H 1.0209 0.5745 0.1891 0.159 Uiso 1 1 calc R . . H15C H 0.9286 0.5810 0.1970 0.159 Uiso 1 1 calc R . . C5 C 0.7954(4) 0.2045(5) 0.1585(3) 0.0552(17) Uani 1 1 d . . . C14 C 0.7215(5) 0.1436(7) 0.1692(5) 0.081(3) Uani 1 1 d . . . H14A H 0.6974 0.1014 0.1343 0.122 Uiso 1 1 calc R . . H14B H 0.6788 0.1898 0.1754 0.122 Uiso 1 1 calc R . . H14C H 0.7414 0.1012 0.2045 0.122 Uiso 1 1 calc R . . C13 C 0.7623(6) 0.2654(7) 0.0993(4) 0.077(2) Uani 1 1 d . . . H13A H 0.8069 0.3083 0.0931 0.115 Uiso 1 1 calc R . . H13B H 0.7151 0.3072 0.1022 0.115 Uiso 1 1 calc R . . H13C H 0.7441 0.2189 0.0657 0.115 Uiso 1 1 calc R . . C4 C 0.8676(4) 0.1337(5) 0.1562(3) 0.0485(15) Uani 1 1 d . . . C3 C 0.8930(6) 0.0886(7) 0.1101(3) 0.069(2) Uani 1 1 d . . . H3 H 0.8748 0.1052 0.0689 0.083 Uiso 1 1 calc R . . C2 C 0.9521(5) 0.0122(6) 0.1369(3) 0.065(2) Uani 1 1 d . . . H2 H 0.9806 -0.0314 0.1168 0.078 Uiso 1 1 calc R . . C1 C 0.9596(4) 0.0142(5) 0.1982(3) 0.0498(15) Uani 1 1 d . . . C11 C 1.0000 -0.0571(7) 0.2500 0.052(2) Uani 1 2 d S . . C12 C 1.0687(6) -0.1251(6) 0.2364(4) 0.074(2) Uani 1 1 d . . . H12A H 1.1150 -0.0833 0.2318 0.110 Uiso 1 1 calc R . . H12B H 1.0452 -0.1625 0.1994 0.110 Uiso 1 1 calc R . . H12C H 1.0892 -0.1723 0.2694 0.110 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 Dy 0.03892(18) 0.04614(19) 0.04102(17) 0.00290(12) 0.01016(12) -0.00029(12) Si1 0.0664(13) 0.0851(16) 0.0501(10) 0.0069(10) 0.0228(10) 0.0114(11) Si2 0.0837(17) 0.0867(17) 0.0600(13) 0.0262(12) 0.0254(12) 0.0125(13) N3 0.060(4) 0.060(4) 0.043(3) 0.007(2) 0.020(3) 0.003(3) N2 0.037(3) 0.040(3) 0.056(3) 0.003(2) 0.005(2) -0.001(2) N1 0.037(3) 0.045(3) 0.047(3) -0.002(2) 0.008(2) 0.000(2) C16 0.155(9) 0.147(8) 0.108(7) -0.031(7) 0.013(6) 0.050(7) C17 0.106(8) 0.152(9) 0.167(9) 0.032(7) 0.056(7) -0.004(7) C18 0.108(7) 0.112(7) 0.095(6) 0.032(5) 0.042(5) 0.029(6) C21 0.139(8) 0.141(8) 0.136(8) 0.050(7) 0.049(7) 0.049(7) C19 0.169(10) 0.156(9) 0.114(8) 0.008(7) 0.012(7) 0.027(8) C20 0.157(9) 0.140(8) 0.162(9) 0.076(7) 0.041(7) -0.025(7) C9 0.050(4) 0.040(4) 0.067(4) 0.001(3) 0.004(3) 0.009(3) C8 0.069(5) 0.056(5) 0.070(5) -0.009(4) 0.013(4) 0.016(4) C7 0.046(4) 0.068(5) 0.074(5) 0.007(4) 0.018(4) 0.013(3) C6 0.042(3) 0.051(4) 0.057(4) 0.011(3) 0.003(3) 0.007(3) C10 0.056(6) 0.040(5) 0.090(8) 0.000 0.000(5) 0.000 C15 0.091(7) 0.054(5) 0.152(10) 0.042(6) -0.002(7) -0.007(5) C5 0.038(3) 0.059(4) 0.059(4) 0.002(3) -0.004(3) -0.003(3) C14 0.039(4) 0.083(6) 0.114(7) 0.002(5) 0.008(4) -0.012(4) C13 0.060(5) 0.084(6) 0.070(5) 0.009(4) -0.012(4) 0.007(4) C4 0.043(3) 0.050(4) 0.047(3) -0.001(3) 0.002(3) -0.005(3) C3 0.073(5) 0.080(6) 0.047(4) -0.006(4) 0.006(4) -0.002(4) C2 0.072(5) 0.068(5) 0.059(4) -0.016(4) 0.022(4) -0.002(4) C1 0.047(4) 0.042(3) 0.060(4) -0.008(3) 0.013(3) -0.005(3) C11 0.053(5) 0.036(5) 0.067(6) 0.000 0.018(5) 0.000 C12 0.073(5) 0.049(4) 0.103(6) -0.002(4) 0.031(5) 0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy N3 2.225(5) . ? Dy N2 2.616(5) . ? Dy N1 2.626(5) 2_755 ? Dy N1 2.646(5) . ? Dy N2 2.680(5) 2_755 ? Dy C6 2.815(6) 2_755 ? Dy C4 2.817(6) . ? Dy C9 2.822(7) 2_755 ? Dy C1 2.834(7) . ? Dy C7 2.930(7) 2_755 ? Dy C8 2.932(7) 2_755 ? Dy C3 2.961(8) . ? Si1 N3 1.715(6) . ? Si1 C16 1.829(12) . ? Si1 C18 1.839(10) . ? Si1 C17 1.859(14) . ? Si2 N3 1.721(6) . ? Si2 C21 1.832(13) . ? Si2 C19 1.840(15) . ? Si2 C20 1.847(13) . ? N2 C9 1.374(9) . ? N2 C6 1.383(9) . ? N2 Dy 2.680(5) 2_755 ? N1 C1 1.380(8) . ? N1 C4 1.385(8) . ? N1 Dy 2.626(5) 2_755 ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C9 C8 1.368(11) . ? C9 C10 1.499(9) . ? C9 Dy 2.822(7) 2_755 ? C8 C7 1.412(11) . ? C8 Dy 2.932(7) 2_755 ? C8 H8 0.9300 . ? C7 C6 1.367(11) . ? C7 Dy 2.930(7) 2_755 ? C7 H7 0.9300 . ? C6 C5 1.508(10) . ? C6 Dy 2.815(6) 2_755 ? C10 C9 1.499(9) 2_755 ? C10 C15 1.543(11) . ? C10 C15 1.543(11) 2_755 ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C5 C4 1.509(10) . ? C5 C14 1.518(10) . ? C5 C13 1.534(10) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C4 C3 1.365(10) . ? C3 C2 1.407(12) . ? C3 H3 0.9300 . ? C2 C1 1.370(10) . ? C2 H2 0.9300 . ? C1 C11 1.508(9) . ? C11 C1 1.508(9) 2_755 ? C11 C12 1.527(9) 2_755 ? C11 C12 1.527(9) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? 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 N3 Dy N2 127.2(2) . . ? N3 Dy N1 129.86(19) . 2_755 ? N2 Dy N1 102.96(17) . 2_755 ? N3 Dy N1 130.30(19) . . ? N2 Dy N1 66.94(17) . . ? N1 Dy N1 66.4(2) 2_755 . ? N3 Dy N2 129.0(2) . 2_755 ? N2 Dy N2 66.7(2) . 2_755 ? N1 Dy N2 66.31(17) 2_755 2_755 ? N1 Dy N2 100.70(16) . 2_755 ? N3 Dy C6 109.5(2) . 2_755 ? N2 Dy C6 95.61(19) . 2_755 ? N1 Dy C6 58.89(19) 2_755 2_755 ? N1 Dy C6 116.39(19) . 2_755 ? N2 Dy C6 29.01(18) 2_755 2_755 ? N3 Dy C4 109.6(2) . . ? N2 Dy C4 59.37(18) . . ? N1 Dy C4 95.46(17) 2_755 . ? N1 Dy C4 29.16(17) . . ? N2 Dy C4 116.71(18) 2_755 . ? C6 Dy C4 140.9(2) 2_755 . ? N3 Dy C9 108.7(2) . 2_755 ? N2 Dy C9 59.12(19) . 2_755 ? N1 Dy C9 94.99(18) 2_755 2_755 ? N1 Dy C9 116.51(19) . 2_755 ? N2 Dy C9 28.78(18) 2_755 2_755 ? C6 Dy C9 45.7(2) 2_755 2_755 ? C4 Dy C9 118.4(2) . 2_755 ? N3 Dy C1 110.6(2) . . ? N2 Dy C1 95.74(18) . . ? N1 Dy C1 59.18(18) 2_755 . ? N1 Dy C1 28.92(17) . . ? N2 Dy C1 116.50(18) 2_755 . ? C6 Dy C1 118.0(2) 2_755 . ? C4 Dy C1 45.77(19) . . ? C9 Dy C1 140.7(2) 2_755 . ? N3 Dy C7 83.8(2) . 2_755 ? N2 Dy C7 104.7(2) . 2_755 ? N1 Dy C7 82.6(2) 2_755 2_755 ? N1 Dy C7 143.8(2) . 2_755 ? N2 Dy C7 47.4(2) 2_755 2_755 ? C6 Dy C7 27.4(2) 2_755 2_755 ? C4 Dy C7 163.2(2) . 2_755 ? C9 Dy C7 45.6(2) 2_755 2_755 ? C1 Dy C7 140.0(2) . 2_755 ? N3 Dy C8 83.4(2) . 2_755 ? N2 Dy C8 82.7(2) . 2_755 ? N1 Dy C8 104.2(2) 2_755 2_755 ? N1 Dy C8 143.9(2) . 2_755 ? N2 Dy C8 47.1(2) 2_755 2_755 ? C6 Dy C8 45.4(2) 2_755 2_755 ? C4 Dy C8 140.5(2) . 2_755 ? C9 Dy C8 27.4(2) 2_755 2_755 ? C1 Dy C8 162.7(2) . 2_755 ? C7 Dy C8 27.9(2) 2_755 2_755 ? N3 Dy C3 84.7(2) . . ? N2 Dy C3 82.9(2) . . ? N1 Dy C3 104.3(2) 2_755 . ? N1 Dy C3 47.10(19) . . ? N2 Dy C3 143.9(2) 2_755 . ? C6 Dy C3 162.5(2) 2_755 . ? C4 Dy C3 27.2(2) . . ? C9 Dy C3 140.6(2) 2_755 . ? C1 Dy C3 45.3(2) . . ? C7 Dy C3 168.5(2) 2_755 . ? C8 Dy C3 150.3(2) 2_755 . ? N3 Si1 C16 115.7(5) . . ? N3 Si1 C18 109.8(4) . . ? C16 Si1 C18 106.4(6) . . ? N3 Si1 C17 114.0(5) . . ? C16 Si1 C17 104.2(8) . . ? C18 Si1 C17 106.0(6) . . ? N3 Si2 C21 110.4(5) . . ? N3 Si2 C19 116.0(6) . . ? C21 Si2 C19 106.8(8) . . ? N3 Si2 C20 113.7(5) . . ? C21 Si2 C20 105.5(8) . . ? C19 Si2 C20 103.6(8) . . ? Si1 N3 Si2 117.6(3) . . ? Si1 N3 Dy 120.3(3) . . ? Si2 N3 Dy 121.9(3) . . ? C9 N2 C6 105.0(6) . . ? C9 N2 Dy 123.2(4) . . ? C6 N2 Dy 122.6(4) . . ? C9 N2 Dy 81.3(4) . 2_755 ? C6 N2 Dy 80.9(4) . 2_755 ? Dy N2 Dy 77.95(14) . 2_755 ? C1 N1 C4 105.2(5) . . ? C1 N1 Dy 123.8(4) . 2_755 ? C4 N1 Dy 123.7(4) . 2_755 ? C1 N1 Dy 83.1(4) . . ? C4 N1 Dy 82.3(4) . . ? Dy N1 Dy 78.38(14) 2_755 . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si1 C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C8 C9 N2 110.6(7) . . ? C8 C9 C10 133.2(7) . . ? N2 C9 C10 115.9(6) . . ? C8 C9 Dy 80.8(5) . 2_755 ? N2 C9 Dy 69.9(3) . 2_755 ? C10 C9 Dy 119.6(4) . 2_755 ? C9 C8 C7 106.9(7) . . ? C9 C8 Dy 71.8(4) . 2_755 ? C7 C8 Dy 76.0(4) . 2_755 ? C9 C8 H8 126.6 . . ? C7 C8 H8 126.6 . . ? Dy C8 H8 117.7 2_755 . ? C6 C7 C8 106.1(7) . . ? C6 C7 Dy 71.6(4) . 2_755 ? C8 C7 Dy 76.1(4) . 2_755 ? C6 C7 H7 127.0 . . ? C8 C7 H7 127.0 . . ? Dy C7 H7 117.5 2_755 . ? C7 C6 N2 110.9(7) . . ? C7 C6 C5 132.3(7) . . ? N2 C6 C5 116.4(6) . . ? C7 C6 Dy 81.0(4) . 2_755 ? N2 C6 Dy 70.1(3) . 2_755 ? C5 C6 Dy 120.4(4) . 2_755 ? C9 C10 C9 103.5(8) . 2_755 ? C9 C10 C15 108.9(5) . . ? C9 C10 C15 113.4(6) 2_755 . ? C9 C10 C15 113.4(6) . 2_755 ? C9 C10 C15 108.9(5) 2_755 2_755 ? C15 C10 C15 108.7(11) . 2_755 ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C6 C5 C4 102.9(5) . . ? C6 C5 C14 113.9(7) . . ? C4 C5 C14 110.3(6) . . ? C6 C5 C13 109.6(6) . . ? C4 C5 C13 112.3(7) . . ? C14 C5 C13 107.9(6) . . ? C5 C14 H14A 109.5 . . ? C5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C5 C13 H13A 109.5 . . ? C5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C4 N1 110.4(6) . . ? C3 C4 C5 133.9(6) . . ? N1 C4 C5 115.2(6) . . ? C3 C4 Dy 82.3(5) . . ? N1 C4 Dy 68.6(3) . . ? C5 C4 Dy 120.4(4) . . ? C4 C3 C2 106.6(7) . . ? C4 C3 Dy 70.5(4) . . ? C2 C3 Dy 76.5(5) . . ? C4 C3 H3 126.7 . . ? C2 C3 H3 126.7 . . ? Dy C3 H3 118.4 . . ? C1 C2 C3 107.0(7) . . ? C1 C2 Dy 71.0(4) . . ? C3 C2 Dy 76.1(5) . . ? C1 C2 H2 126.5 . . ? C3 C2 H2 126.5 . . ? Dy C2 H2 118.4 . . ? C2 C1 N1 110.1(6) . . ? C2 C1 C11 133.4(6) . . ? N1 C1 C11 116.2(6) . . ? C2 C1 Dy 81.8(5) . . ? N1 C1 Dy 68.0(3) . . ? C11 C1 Dy 119.7(4) . . ? C1 C11 C1 103.8(7) 2_755 . ? C1 C11 C12 112.9(4) 2_755 2_755 ? C1 C11 C12 109.2(4) . 2_755 ? C1 C11 C12 109.2(4) 2_755 . ? C1 C11 C12 112.9(4) . . ? C12 C11 C12 108.8(9) 2_755 . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Si1 N3 Si2 -57.0(7) . . . . ? C18 Si1 N3 Si2 -177.4(5) . . . . ? C17 Si1 N3 Si2 63.8(7) . . . . ? C16 Si1 N3 Dy 127.4(6) . . . . ? C18 Si1 N3 Dy 7.0(6) . . . . ? C17 Si1 N3 Dy -111.7(7) . . . . ? C21 Si2 N3 Si1 176.8(7) . . . . ? C19 Si2 N3 Si1 55.1(8) . . . . ? C20 Si2 N3 Si1 -64.9(7) . . . . ? C21 Si2 N3 Dy -7.7(7) . . . . ? C19 Si2 N3 Dy -129.4(7) . . . . ? C20 Si2 N3 Dy 110.6(7) . . . . ? N2 Dy N3 Si1 176.3(3) . . . . ? N1 Dy N3 Si1 -2.4(5) 2_755 . . . ? N1 Dy N3 Si1 -93.8(4) . . . . ? N2 Dy N3 Si1 87.7(4) 2_755 . . . ? C6 Dy N3 Si1 62.8(4) 2_755 . . . ? C4 Dy N3 Si1 -117.8(4) . . . . ? C9 Dy N3 Si1 111.3(4) 2_755 . . . ? C1 Dy N3 Si1 -68.9(4) . . . . ? C7 Dy N3 Si1 72.6(4) 2_755 . . . ? C8 Dy N3 Si1 100.6(4) 2_755 . . . ? C3 Dy N3 Si1 -106.7(4) . . . . ? N2 Dy N3 Si2 0.9(5) . . . . ? N1 Dy N3 Si2 -177.8(3) 2_755 . . . ? N1 Dy N3 Si2 90.9(4) . . . . ? N2 Dy N3 Si2 -87.6(4) 2_755 . . . ? C6 Dy N3 Si2 -112.5(4) 2_755 . . . ? C4 Dy N3 Si2 66.8(4) . . . . ? C9 Dy N3 Si2 -64.0(4) 2_755 . . . ? C1 Dy N3 Si2 115.8(4) . . . . ? C7 Dy N3 Si2 -102.8(4) 2_755 . . . ? C8 Dy N3 Si2 -74.7(4) 2_755 . . . ? C3 Dy N3 Si2 77.9(4) . . . . ? N3 Dy N2 C9 -107.9(5) . . . . ? N1 Dy N2 C9 71.1(5) 2_755 . . . ? N1 Dy N2 C9 128.1(5) . . . . ? N2 Dy N2 C9 14.4(5) 2_755 . . . ? C6 Dy N2 C9 11.8(5) 2_755 . . . ? C4 Dy N2 C9 159.8(6) . . . . ? C9 Dy N2 C9 -16.9(6) 2_755 . . . ? C1 Dy N2 C9 130.8(5) . . . . ? C7 Dy N2 C9 -14.5(6) 2_755 . . . ? C8 Dy N2 C9 -31.8(5) 2_755 . . . ? C3 Dy N2 C9 174.3(5) . . . . ? N3 Dy N2 C6 110.2(5) . . . . ? N1 Dy N2 C6 -70.8(5) 2_755 . . . ? N1 Dy N2 C6 -13.8(5) . . . . ? N2 Dy N2 C6 -127.5(6) 2_755 . . . ? C6 Dy N2 C6 -130.1(4) 2_755 . . . ? C4 Dy N2 C6 17.9(5) . . . . ? C9 Dy N2 C6 -158.9(6) 2_755 . . . ? C1 Dy N2 C6 -11.1(5) . . . . ? C7 Dy N2 C6 -156.5(5) 2_755 . . . ? C8 Dy N2 C6 -173.8(5) 2_755 . . . ? C3 Dy N2 C6 32.4(5) . . . . ? N3 Dy N2 Dy -178.9(2) . . . 2_755 ? N1 Dy N2 Dy 0.04(16) 2_755 . . 2_755 ? N1 Dy N2 Dy 57.04(14) . . . 2_755 ? N2 Dy N2 Dy -56.72(18) 2_755 . . 2_755 ? C6 Dy N2 Dy -59.29(18) 2_755 . . 2_755 ? C4 Dy N2 Dy 88.73(19) . . . 2_755 ? C9 Dy N2 Dy -88.0(2) 2_755 . . 2_755 ? C1 Dy N2 Dy 59.69(17) . . . 2_755 ? C7 Dy N2 Dy -85.63(19) 2_755 . . 2_755 ? C8 Dy N2 Dy -102.93(19) 2_755 . . 2_755 ? C3 Dy N2 Dy 103.20(19) . . . 2_755 ? N3 Dy N1 C1 54.5(4) . . . . ? N2 Dy N1 C1 174.5(4) . . . . ? N1 Dy N1 C1 -68.6(3) 2_755 . . . ? N2 Dy N1 C1 -126.6(4) 2_755 . . . ? C6 Dy N1 C1 -100.8(4) 2_755 . . . ? C4 Dy N1 C1 106.5(5) . . . . ? C9 Dy N1 C1 -152.2(4) 2_755 . . . ? C7 Dy N1 C1 -102.1(5) 2_755 . . . ? C8 Dy N1 C1 -150.3(4) 2_755 . . . ? C3 Dy N1 C1 72.2(4) . . . . ? N3 Dy N1 C4 -51.9(4) . . . . ? N2 Dy N1 C4 68.1(4) . . . . ? N1 Dy N1 C4 -175.1(4) 2_755 . . . ? N2 Dy N1 C4 126.9(4) 2_755 . . . ? C6 Dy N1 C4 152.8(4) 2_755 . . . ? C9 Dy N1 C4 101.4(4) 2_755 . . . ? C1 Dy N1 C4 -106.5(5) . . . . ? C7 Dy N1 C4 151.5(4) 2_755 . . . ? C8 Dy N1 C4 103.3(5) 2_755 . . . ? C3 Dy N1 C4 -34.2(4) . . . . ? N3 Dy N1 Dy -178.8(2) . . . 2_755 ? N2 Dy N1 Dy -58.77(15) . . . 2_755 ? N1 Dy N1 Dy 58.11(18) 2_755 . . 2_755 ? N2 Dy N1 Dy 0.04(15) 2_755 . . 2_755 ? C6 Dy N1 Dy 25.9(2) 2_755 . . 2_755 ? C4 Dy N1 Dy -126.8(4) . . . 2_755 ? C9 Dy N1 Dy -25.5(2) 2_755 . . 2_755 ? C1 Dy N1 Dy 126.7(4) . . . 2_755 ? C7 Dy N1 Dy 24.6(4) 2_755 . . 2_755 ? C8 Dy N1 Dy -23.6(4) 2_755 . . 2_755 ? C3 Dy N1 Dy -161.1(3) . . . 2_755 ? C6 N2 C9 C8 6.8(8) . . . . ? Dy N2 C9 C8 -140.7(5) . . . . ? Dy N2 C9 C8 -71.3(6) 2_755 . . . ? C6 N2 C9 C10 -167.8(5) . . . . ? Dy N2 C9 C10 44.7(7) . . . . ? Dy N2 C9 C10 114.1(5) 2_755 . . . ? C6 N2 C9 Dy 78.1(4) . . . 2_755 ? Dy N2 C9 Dy -69.4(4) . . . 2_755 ? N2 C9 C8 C7 -4.2(8) . . . . ? C10 C9 C8 C7 169.1(7) . . . . ? Dy C9 C8 C7 -68.5(5) 2_755 . . . ? N2 C9 C8 Dy 64.3(5) . . . 2_755 ? C10 C9 C8 Dy -122.3(8) . . . 2_755 ? C9 C8 C7 C6 -0.1(9) . . . . ? Dy C8 C7 C6 -65.8(5) 2_755 . . . ? C9 C8 C7 Dy 65.7(5) . . . 2_755 ? C8 C7 C6 N2 4.4(8) . . . . ? Dy C7 C6 N2 -64.5(5) 2_755 . . . ? C8 C7 C6 C5 -167.8(7) . . . . ? Dy C7 C6 C5 123.2(8) 2_755 . . . ? C8 C7 C6 Dy 69.0(5) . . . 2_755 ? C9 N2 C6 C7 -6.9(7) . . . . ? Dy N2 C6 C7 140.8(5) . . . . ? Dy N2 C6 C7 71.5(5) 2_755 . . . ? C9 N2 C6 C5 166.7(6) . . . . ? Dy N2 C6 C5 -45.6(7) . . . . ? Dy N2 C6 C5 -114.9(5) 2_755 . . . ? C9 N2 C6 Dy -78.4(4) . . . 2_755 ? Dy N2 C6 Dy 69.3(3) . . . 2_755 ? C8 C9 C10 C9 139.3(10) . . . 2_755 ? N2 C9 C10 C9 -47.7(4) . . . 2_755 ? Dy C9 C10 C9 32.9(2) 2_755 . . 2_755 ? C8 C9 C10 C15 -99.8(10) . . . . ? N2 C9 C10 C15 73.3(9) . . . . ? Dy C9 C10 C15 153.9(6) 2_755 . . . ? C8 C9 C10 C15 21.4(11) . . . 2_755 ? N2 C9 C10 C15 -165.6(7) . . . 2_755 ? Dy C9 C10 C15 -85.0(7) 2_755 . . 2_755 ? C7 C6 C5 C4 -141.0(8) . . . . ? N2 C6 C5 C4 47.0(7) . . . . ? Dy C6 C5 C4 -34.4(7) 2_755 . . . ? C7 C6 C5 C14 -21.7(11) . . . . ? N2 C6 C5 C14 166.4(6) . . . . ? Dy C6 C5 C14 85.0(7) 2_755 . . . ? C7 C6 C5 C13 99.3(10) . . . . ? N2 C6 C5 C13 -72.7(8) . . . . ? Dy C6 C5 C13 -154.1(5) 2_755 . . . ? C1 N1 C4 C3 -8.1(8) . . . . ? Dy N1 C4 C3 143.0(5) 2_755 . . . ? Dy N1 C4 C3 72.5(6) . . . . ? C1 N1 C4 C5 164.8(5) . . . . ? Dy N1 C4 C5 -44.1(7) 2_755 . . . ? Dy N1 C4 C5 -114.5(5) . . . . ? C1 N1 C4 Dy -80.6(4) . . . . ? Dy N1 C4 Dy 70.4(3) 2_755 . . . ? C6 C5 C4 C3 -141.6(8) . . . . ? C14 C5 C4 C3 96.6(10) . . . . ? C13 C5 C4 C3 -23.8(11) . . . . ? C6 C5 C4 N1 47.7(7) . . . . ? C14 C5 C4 N1 -74.2(8) . . . . ? C13 C5 C4 N1 165.5(6) . . . . ? C6 C5 C4 Dy -31.2(7) . . . . ? C14 C5 C4 Dy -153.1(5) . . . . ? C13 C5 C4 Dy 86.6(6) . . . . ? N3 Dy C4 C3 24.8(5) . . . . ? N2 Dy C4 C3 147.1(5) . . . . ? N1 Dy C4 C3 -111.0(5) 2_755 . . . ? N1 Dy C4 C3 -115.6(6) . . . . ? N2 Dy C4 C3 -177.2(4) 2_755 . . . ? C6 Dy C4 C3 -156.1(4) 2_755 . . . ? C9 Dy C4 C3 150.3(5) 2_755 . . . ? C1 Dy C4 C3 -75.2(5) . . . . ? C7 Dy C4 C3 166.4(7) 2_755 . . . ? C8 Dy C4 C3 128.8(5) 2_755 . . . ? N3 Dy C4 N1 140.4(4) . . . . ? N2 Dy C4 N1 -97.3(4) . . . . ? N1 Dy C4 N1 4.6(4) 2_755 . . . ? N2 Dy C4 N1 -61.6(4) 2_755 . . . ? C6 Dy C4 N1 -40.6(5) 2_755 . . . ? C9 Dy C4 N1 -94.1(4) 2_755 . . . ? C1 Dy C4 N1 40.3(3) . . . . ? C7 Dy C4 N1 -78.0(8) 2_755 . . . ? C8 Dy C4 N1 -115.7(4) 2_755 . . . ? C3 Dy C4 N1 115.6(6) . . . . ? N3 Dy C4 C5 -112.2(5) . . . . ? N2 Dy C4 C5 10.1(5) . . . . ? N1 Dy C4 C5 112.0(5) 2_755 . . . ? N1 Dy C4 C5 107.4(6) . . . . ? N2 Dy C4 C5 45.8(5) 2_755 . . . ? C6 Dy C4 C5 66.8(6) 2_755 . . . ? C9 Dy C4 C5 13.3(6) 2_755 . . . ? C1 Dy C4 C5 147.7(6) . . . . ? C7 Dy C4 C5 29.4(10) 2_755 . . . ? C8 Dy C4 C5 -8.2(7) 2_755 . . . ? C3 Dy C4 C5 -137.0(8) . . . . ? N1 C4 C3 C2 5.0(9) . . . . ? C5 C4 C3 C2 -166.1(8) . . . . ? Dy C4 C3 C2 68.6(6) . . . . ? N1 C4 C3 Dy -63.6(5) . . . . ? C5 C4 C3 Dy 125.3(8) . . . . ? N3 Dy C3 C4 -156.6(5) . . . . ? N2 Dy C3 C4 -28.1(4) . . . . ? N1 Dy C3 C4 73.6(5) 2_755 . . . ? N1 Dy C3 C4 36.9(4) . . . . ? N2 Dy C3 C4 4.3(7) 2_755 . . . ? C6 Dy C3 C4 58.2(10) 2_755 . . . ? C9 Dy C3 C4 -43.3(6) 2_755 . . . ? C1 Dy C3 C4 77.3(5) . . . . ? C7 Dy C3 C4 -160.2(10) 2_755 . . . ? C8 Dy C3 C4 -89.8(6) 2_755 . . . ? N3 Dy C3 C2 90.0(5) . . . . ? N2 Dy C3 C2 -141.4(5) . . . . ? N1 Dy C3 C2 -39.8(5) 2_755 . . . ? N1 Dy C3 C2 -76.5(5) . . . . ? N2 Dy C3 C2 -109.1(5) 2_755 . . . ? C6 Dy C3 C2 -55.2(10) 2_755 . . . ? C4 Dy C3 C2 -113.4(7) . . . . ? C9 Dy C3 C2 -156.7(4) 2_755 . . . ? C1 Dy C3 C2 -36.1(4) . . . . ? C7 Dy C3 C2 86.4(12) 2_755 . . . ? C8 Dy C3 C2 156.8(5) 2_755 . . . ? C4 C3 C2 C1 0.2(9) . . . . ? Dy C3 C2 C1 64.8(5) . . . . ? C4 C3 C2 Dy -64.6(5) . . . . ? N3 Dy C2 C1 158.7(5) . . . . ? N2 Dy C2 C1 -74.1(5) . . . . ? N1 Dy C2 C1 27.5(5) 2_755 . . . ? N1 Dy C2 C1 -36.6(4) . . . . ? N2 Dy C2 C1 -4.0(7) 2_755 . . . ? C6 Dy C2 C1 43.6(6) 2_755 . . . ? C4 Dy C2 C1 -77.5(5) . . . . ? C9 Dy C2 C1 -56.5(10) 2_755 . . . ? C7 Dy C2 C1 89.5(6) 2_755 . . . ? C8 Dy C2 C1 157.4(10) 2_755 . . . ? C3 Dy C2 C1 -113.8(7) . . . . ? N3 Dy C2 C3 -87.5(5) . . . . ? N2 Dy C2 C3 39.7(5) . . . . ? N1 Dy C2 C3 141.3(5) 2_755 . . . ? N1 Dy C2 C3 77.2(5) . . . . ? N2 Dy C2 C3 109.8(5) 2_755 . . . ? C6 Dy C2 C3 157.4(5) 2_755 . . . ? C4 Dy C2 C3 36.3(4) . . . . ? C9 Dy C2 C3 57.3(9) 2_755 . . . ? C1 Dy C2 C3 113.8(7) . . . . ? C7 Dy C2 C3 -156.7(5) 2_755 . . . ? C8 Dy C2 C3 -88.8(13) 2_755 . . . ? C3 C2 C1 N1 -5.3(9) . . . . ? Dy C2 C1 N1 62.9(4) . . . . ? C3 C2 C1 C11 168.2(7) . . . . ? Dy C2 C1 C11 -123.6(8) . . . . ? C3 C2 C1 Dy -68.2(6) . . . . ? C4 N1 C1 C2 8.2(7) . . . . ? Dy N1 C1 C2 -142.8(5) 2_755 . . . ? Dy N1 C1 C2 -71.8(5) . . . . ? C4 N1 C1 C11 -166.6(5) . . . . ? Dy N1 C1 C11 42.4(7) 2_755 . . . ? Dy N1 C1 C11 113.4(5) . . . . ? C4 N1 C1 Dy 80.0(4) . . . . ? Dy N1 C1 Dy -71.0(3) 2_755 . . . ? N3 Dy C1 C2 -22.8(5) . . . . ? N2 Dy C1 C2 110.6(5) . . . . ? N1 Dy C1 C2 -147.7(5) 2_755 . . . ? N1 Dy C1 C2 115.6(6) . . . . ? N2 Dy C1 C2 177.4(4) 2_755 . . . ? C6 Dy C1 C2 -149.9(5) 2_755 . . . ? C4 Dy C1 C2 74.9(5) . . . . ? C9 Dy C1 C2 156.9(4) 2_755 . . . ? C7 Dy C1 C2 -128.3(5) 2_755 . . . ? C8 Dy C1 C2 -165.4(7) 2_755 . . . ? C3 Dy C1 C2 36.5(5) . . . . ? N3 Dy C1 N1 -138.4(4) . . . . ? N2 Dy C1 N1 -5.0(4) . . . . ? N1 Dy C1 N1 96.6(4) 2_755 . . . ? N2 Dy C1 N1 61.8(4) 2_755 . . . ? C6 Dy C1 N1 94.4(4) 2_755 . . . ? C4 Dy C1 N1 -40.7(3) . . . . ? C9 Dy C1 N1 41.2(5) 2_755 . . . ? C7 Dy C1 N1 116.1(4) 2_755 . . . ? C8 Dy C1 N1 78.9(8) 2_755 . . . ? C3 Dy C1 N1 -79.2(4) . . . . ? N3 Dy C1 C11 113.0(4) . . . . ? N2 Dy C1 C11 -113.6(4) . . . . ? N1 Dy C1 C11 -11.9(4) 2_755 . . . ? N1 Dy C1 C11 -108.6(6) . . . . ? N2 Dy C1 C11 -46.8(5) 2_755 . . . ? C6 Dy C1 C11 -14.1(5) 2_755 . . . ? C4 Dy C1 C11 -149.3(6) . . . . ? C9 Dy C1 C11 -67.3(5) 2_755 . . . ? C7 Dy C1 C11 7.5(6) 2_755 . . . ? C8 Dy C1 C11 -29.6(10) 2_755 . . . ? C3 Dy C1 C11 172.3(6) . . . . ? C2 C1 C11 C1 140.8(9) . . . 2_755 ? N1 C1 C11 C1 -46.0(4) . . . 2_755 ? Dy C1 C11 C1 32.52(18) . . . 2_755 ? C2 C1 C11 C12 -98.5(9) . . . 2_755 ? N1 C1 C11 C12 74.7(7) . . . 2_755 ? Dy C1 C11 C12 153.2(5) . . . 2_755 ? C2 C1 C11 C12 22.7(11) . . . . ? N1 C1 C11 C12 -164.1(6) . . . . ? Dy C1 C11 C12 -85.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.378 _refine_diff_density_min -1.359 _refine_diff_density_rms 0.166 # Attachment '4906_web_deposit_cif_file_3_ShuangliuZhou_1301667625.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 819830' #TrackingRef '4906_web_deposit_cif_file_3_ShuangliuZhou_1301667625.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H84 N6 Nd2 Si4' _chemical_formula_weight 1230.12 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' Nd Nd -0.1943 3.0179 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6462(7) _cell_length_b 29.2019(15) _cell_length_c 16.5042(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.5910(10) _cell_angle_gamma 90.00 _cell_volume 6041.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 1.817 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7722 _exptl_absorpt_correction_T_max 0.8115 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52146 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.54 _reflns_number_total 13934 _reflns_number_gt 11599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+4.4158P] 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 13934 _refine_ls_number_parameters 616 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0614 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.003 _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 Nd2 Nd 0.884989(11) 0.147089(5) 0.735271(8) 0.02992(4) Uani 1 1 d . . . Nd1 Nd 0.826530(11) 0.137520(5) 0.934953(9) 0.03116(4) Uani 1 1 d . . . Si1 Si 0.85317(8) 0.17040(4) 1.14208(5) 0.0545(2) Uani 1 1 d . . . Si2 Si 0.70672(8) 0.09264(4) 1.09734(6) 0.0544(2) Uani 1 1 d . . . Si3 Si 1.00749(8) 0.12014(4) 0.56422(6) 0.0594(3) Uani 1 1 d . . . Si4 Si 0.85914(8) 0.19986(4) 0.54300(6) 0.0614(3) Uani 1 1 d . . . N1 N 0.74464(17) 0.19463(8) 0.80963(13) 0.0342(5) Uani 1 1 d . . . N2 N 0.73480(16) 0.09267(7) 0.79790(13) 0.0315(5) Uani 1 1 d . . . N3 N 0.96917(16) 0.08915(7) 0.85542(13) 0.0296(5) Uani 1 1 d . . . N4 N 0.97418(17) 0.18994(7) 0.87601(13) 0.0320(5) Uani 1 1 d . . . N5 N 0.7928(2) 0.13324(9) 1.06984(15) 0.0476(6) Uani 1 1 d . . . N6 N 0.91964(19) 0.15638(10) 0.60162(14) 0.0471(6) Uani 1 1 d . . . C1 C 0.8646(2) 0.25893(9) 0.85237(17) 0.0382(6) Uani 1 1 d . . . C2 C 0.8186(3) 0.29406(10) 0.78664(19) 0.0463(7) Uani 1 1 d . . . H2A H 0.7978 0.2779 0.7357 0.056 Uiso 1 1 calc R . . H2B H 0.7546 0.3074 0.8033 0.056 Uiso 1 1 calc R . . C3 C 0.8944(3) 0.33255(11) 0.7711(2) 0.0553(8) Uani 1 1 d . . . H3A H 0.9522 0.3201 0.7446 0.066 Uiso 1 1 calc R . . H3B H 0.8566 0.3547 0.7343 0.066 Uiso 1 1 calc R . . C4 C 0.9405(3) 0.35643(12) 0.8495(2) 0.0663(10) Uani 1 1 d . . . H4A H 0.8843 0.3728 0.8720 0.080 Uiso 1 1 calc R . . H4B H 0.9938 0.3785 0.8379 0.080 Uiso 1 1 calc R . . C5 C 0.9909(3) 0.32170(12) 0.9115(2) 0.0595(9) Uani 1 1 d . . . H5A H 1.0502 0.3068 0.8904 0.071 Uiso 1 1 calc R . . H5B H 1.0184 0.3373 0.9617 0.071 Uiso 1 1 calc R . . C6 C 0.9102(3) 0.28583(11) 0.92940(19) 0.0492(8) Uani 1 1 d . . . H6A H 0.8522 0.3007 0.9521 0.059 Uiso 1 1 calc R . . H6B H 0.9441 0.2646 0.9700 0.059 Uiso 1 1 calc R . . C7 C 0.7765(2) 0.22723(9) 0.86859(17) 0.0378(6) Uani 1 1 d . . . C8 C 0.7113(2) 0.22583(11) 0.92960(19) 0.0462(7) Uani 1 1 d . . . H8 H 0.7188 0.2431 0.9774 0.055 Uiso 1 1 calc R . . C9 C 0.6308(2) 0.19289(11) 0.90510(18) 0.0451(7) Uani 1 1 d . . . H9 H 0.5753 0.1845 0.9337 0.054 Uiso 1 1 calc R . . C10 C 0.6509(2) 0.17570(10) 0.83039(17) 0.0368(6) Uani 1 1 d . . . C11 C 0.5877(2) 0.14664(10) 0.76755(17) 0.0369(6) Uani 1 1 d . . . C12 C 0.5040(2) 0.11718(12) 0.80395(18) 0.0468(7) Uani 1 1 d . . . H12A H 0.5405 0.0953 0.8420 0.056 Uiso 1 1 calc R . . H12B H 0.4613 0.1368 0.8342 0.056 Uiso 1 1 calc R . . C13 C 0.4311(3) 0.09162(14) 0.7389(2) 0.0613(10) Uani 1 1 d . . . H13A H 0.4732 0.0707 0.7105 0.074 Uiso 1 1 calc R . . H13B H 0.3804 0.0736 0.7647 0.074 Uiso 1 1 calc R . . C14 C 0.3715(3) 0.12427(16) 0.6781(2) 0.0731(12) Uani 1 1 d . . . H14A H 0.3247 0.1434 0.7056 0.088 Uiso 1 1 calc R . . H14B H 0.3277 0.1070 0.6361 0.088 Uiso 1 1 calc R . . C15 C 0.4489(3) 0.15436(14) 0.6385(2) 0.0637(10) Uani 1 1 d . . . H15A H 0.4879 0.1356 0.6040 0.076 Uiso 1 1 calc R . . H15B H 0.4091 0.1771 0.6043 0.076 Uiso 1 1 calc R . . C16 C 0.5273(2) 0.17826(12) 0.70238(19) 0.0499(8) Uani 1 1 d . . . H16A H 0.4888 0.2010 0.7299 0.060 Uiso 1 1 calc R . . H16B H 0.5792 0.1944 0.6747 0.060 Uiso 1 1 calc R . . C17 C 0.6692(2) 0.11528(9) 0.73697(16) 0.0330(6) Uani 1 1 d . . . C18 C 0.6910(2) 0.10141(10) 0.66118(17) 0.0383(6) Uani 1 1 d . . . H18 H 0.6613 0.1130 0.6108 0.046 Uiso 1 1 calc R . . C19 C 0.7680(2) 0.06584(10) 0.67503(17) 0.0380(6) Uani 1 1 d . . . H19 H 0.7980 0.0495 0.6354 0.046 Uiso 1 1 calc R . . C20 C 0.7894(2) 0.06020(9) 0.75839(16) 0.0332(6) Uani 1 1 d . . . C21 C 0.8491(2) 0.02522(9) 0.81388(16) 0.0328(6) Uani 1 1 d . . . C22 C 0.7690(2) -0.00786(10) 0.84584(18) 0.0408(7) Uani 1 1 d . . . H22A H 0.8055 -0.0253 0.8912 0.049 Uiso 1 1 calc R . . H22B H 0.7132 0.0098 0.8662 0.049 Uiso 1 1 calc R . . C23 C 0.7187(3) -0.04079(12) 0.7808(2) 0.0561(9) Uani 1 1 d . . . H23A H 0.6775 -0.0236 0.7373 0.067 Uiso 1 1 calc R . . H23B H 0.6702 -0.0610 0.8045 0.067 Uiso 1 1 calc R . . C24 C 0.8022(3) -0.06925(12) 0.7454(2) 0.0634(10) Uani 1 1 d . . . H24A H 0.7675 -0.0889 0.7025 0.076 Uiso 1 1 calc R . . H24B H 0.8393 -0.0886 0.7878 0.076 Uiso 1 1 calc R . . C25 C 0.8819(3) -0.03830(11) 0.7107(2) 0.0535(8) Uani 1 1 d . . . H25A H 0.8463 -0.0220 0.6636 0.064 Uiso 1 1 calc R . . H25B H 0.9380 -0.0568 0.6927 0.064 Uiso 1 1 calc R . . C26 C 0.9310(2) -0.00390(10) 0.77413(19) 0.0424(7) Uani 1 1 d . . . H26A H 0.9769 0.0166 0.7483 0.051 Uiso 1 1 calc R . . H26B H 0.9755 -0.0203 0.8169 0.051 Uiso 1 1 calc R . . C27 C 0.9105(2) 0.05317(9) 0.88091(16) 0.0311(5) Uani 1 1 d . . . C28 C 0.9296(2) 0.04833(9) 0.96413(17) 0.0362(6) Uani 1 1 d . . . H28 H 0.8963 0.0279 0.9959 0.043 Uiso 1 1 calc R . . C29 C 1.0102(2) 0.08062(9) 0.99230(17) 0.0361(6) Uani 1 1 d . . . H29 H 1.0401 0.0854 1.0462 0.043 Uiso 1 1 calc R . . C30 C 1.03566(19) 0.10348(9) 0.92436(16) 0.0310(5) Uani 1 1 d . . . C31 C 1.1226(2) 0.13611(9) 0.90709(16) 0.0323(6) Uani 1 1 d . . . C32 C 1.2076(2) 0.10929(10) 0.86779(18) 0.0405(7) Uani 1 1 d . . . H32A H 1.1725 0.0905 0.8237 0.049 Uiso 1 1 calc R . . H32B H 1.2538 0.1308 0.8445 0.049 Uiso 1 1 calc R . . C33 C 1.2750(2) 0.07877(12) 0.9290(2) 0.0532(8) Uani 1 1 d . . . H33A H 1.2295 0.0560 0.9498 0.064 Uiso 1 1 calc R . . H33B H 1.3274 0.0628 0.9016 0.064 Uiso 1 1 calc R . . C34 C 1.3317(3) 0.10613(14) 0.9997(2) 0.0632(10) Uani 1 1 d . . . H34A H 1.3715 0.0855 1.0385 0.076 Uiso 1 1 calc R . . H34B H 1.3819 0.1270 0.9796 0.076 Uiso 1 1 calc R . . C35 C 1.2527(3) 0.13303(12) 1.0421(2) 0.0549(8) Uani 1 1 d . . . H35A H 1.2912 0.1527 1.0833 0.066 Uiso 1 1 calc R . . H35B H 1.2098 0.1120 1.0695 0.066 Uiso 1 1 calc R . . C36 C 1.1799(2) 0.16223(11) 0.98154(18) 0.0436(7) Uani 1 1 d . . . H36A H 1.2220 0.1866 0.9619 0.052 Uiso 1 1 calc R . . H36B H 1.1264 0.1764 1.0104 0.052 Uiso 1 1 calc R . . C37 C 1.0657(2) 0.17140(9) 0.85147(16) 0.0324(6) Uani 1 1 d . . . C38 C 1.0910(2) 0.19374(10) 0.78268(17) 0.0389(6) Uani 1 1 d . . . H38 H 1.1461 0.1865 0.7527 0.047 Uiso 1 1 calc R . . C39 C 1.0163(2) 0.22998(10) 0.76683(18) 0.0413(7) Uani 1 1 d . . . H39 H 1.0130 0.2511 0.7245 0.050 Uiso 1 1 calc R . . C40 C 0.9493(2) 0.22774(9) 0.82630(16) 0.0342(6) Uani 1 1 d . . . C41 C 0.9721(4) 0.19669(15) 1.1042(3) 0.0859(14) Uani 1 1 d . . . H41A H 1.0326 0.1769 1.1169 0.129 Uiso 1 1 calc R . . H41B H 0.9869 0.2258 1.1302 0.129 Uiso 1 1 calc R . . H41C H 0.9578 0.2009 1.0461 0.129 Uiso 1 1 calc R . . C42 C 0.9068(4) 0.14252(16) 1.2403(2) 0.0868(14) Uani 1 1 d . . . H42A H 0.8489 0.1303 1.2657 0.130 Uiso 1 1 calc R . . H42B H 0.9448 0.1647 1.2759 0.130 Uiso 1 1 calc R . . H42C H 0.9542 0.1182 1.2299 0.130 Uiso 1 1 calc R . . C43 C 0.7658(4) 0.21841(17) 1.1679(3) 0.1025(17) Uani 1 1 d . . . H43A H 0.7556 0.2397 1.1232 0.154 Uiso 1 1 calc R . . H43B H 0.7989 0.2338 1.2161 0.154 Uiso 1 1 calc R . . H43C H 0.6979 0.2064 1.1777 0.154 Uiso 1 1 calc R . . C44 C 0.7735(3) 0.04421(15) 1.1595(3) 0.0811(13) Uani 1 1 d . . . H44A H 0.8242 0.0297 1.1294 0.122 Uiso 1 1 calc R . . H44B H 0.7208 0.0223 1.1707 0.122 Uiso 1 1 calc R . . H44C H 0.8097 0.0559 1.2100 0.122 Uiso 1 1 calc R . . C45 C 0.6016(3) 0.11643(19) 1.1552(3) 0.0961(16) Uani 1 1 d . . . H45A H 0.6342 0.1274 1.2075 0.144 Uiso 1 1 calc R . . H45B H 0.5510 0.0929 1.1630 0.144 Uiso 1 1 calc R . . H45C H 0.5658 0.1413 1.1249 0.144 Uiso 1 1 calc R . . C46 C 0.6343(3) 0.06543(16) 1.0033(2) 0.0777(12) Uani 1 1 d . . . H46A H 0.5807 0.0861 0.9781 0.117 Uiso 1 1 calc R . . H46B H 0.6011 0.0376 1.0180 0.117 Uiso 1 1 calc R . . H46C H 0.6840 0.0587 0.9657 0.117 Uiso 1 1 calc R . . C47 C 1.0747(3) 0.08487(14) 0.6505(2) 0.0695(11) Uani 1 1 d . . . H47A H 1.1286 0.1029 0.6823 0.104 Uiso 1 1 calc R . . H47B H 1.1070 0.0585 0.6291 0.104 Uiso 1 1 calc R . . H47C H 1.0230 0.0751 0.6845 0.104 Uiso 1 1 calc R . . C48 C 1.1147(4) 0.1498(2) 0.5166(3) 0.117(2) Uani 1 1 d . . . H48A H 1.0831 0.1683 0.4717 0.176 Uiso 1 1 calc R . . H48B H 1.1609 0.1274 0.4970 0.176 Uiso 1 1 calc R . . H48C H 1.1554 0.1689 0.5565 0.176 Uiso 1 1 calc R . . C49 C 0.9433(4) 0.0789(2) 0.4864(3) 0.118(2) Uani 1 1 d . . . H49A H 0.8949 0.0596 0.5108 0.177 Uiso 1 1 calc R . . H49B H 0.9972 0.0604 0.4665 0.177 Uiso 1 1 calc R . . H49C H 0.9048 0.0955 0.4417 0.177 Uiso 1 1 calc R . . C50 C 0.9472(4) 0.25137(19) 0.5363(4) 0.128(2) Uani 1 1 d . . . H50A H 0.9580 0.2666 0.5883 0.192 Uiso 1 1 calc R . . H50B H 0.9138 0.2720 0.4955 0.192 Uiso 1 1 calc R . . H50C H 1.0148 0.2417 0.5218 0.192 Uiso 1 1 calc R . . C51 C 0.7411(3) 0.22062(13) 0.5878(2) 0.0672(10) Uani 1 1 d . . . H51A H 0.6813 0.2011 0.5707 0.101 Uiso 1 1 calc R . . H51B H 0.7246 0.2513 0.5696 0.101 Uiso 1 1 calc R . . H51C H 0.7563 0.2202 0.6464 0.101 Uiso 1 1 calc R . . C52 C 0.8087(4) 0.1837(2) 0.4365(2) 0.138(3) Uani 1 1 d . . . H52A H 0.8678 0.1781 0.4069 0.207 Uiso 1 1 calc R . . H52B H 0.7658 0.2081 0.4108 0.207 Uiso 1 1 calc R . . H52C H 0.7663 0.1564 0.4366 0.207 Uiso 1 1 calc R . . C53 C 0.479(2) 0.9908(11) 0.5391(14) 0.320(11) Uani 1 1 d . . . C54 C 0.369(3) 1.0142(11) 0.5153(17) 0.416(15) Uani 1 1 d . . . C55 C 0.362(3) 0.9746(7) 0.5871(15) 0.406(17) 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 Nd2 0.03028(7) 0.03267(8) 0.02766(7) 0.00314(6) 0.00701(5) 0.00145(5) Nd1 0.03218(8) 0.03390(8) 0.02852(7) 0.00239(6) 0.00820(6) 0.00464(6) Si1 0.0681(6) 0.0618(6) 0.0358(5) -0.0035(4) 0.0154(4) 0.0157(5) Si2 0.0510(5) 0.0777(7) 0.0366(5) 0.0055(4) 0.0134(4) 0.0089(5) Si3 0.0552(6) 0.0879(8) 0.0381(5) 0.0059(5) 0.0171(4) 0.0028(5) Si4 0.0482(5) 0.0983(8) 0.0396(5) 0.0238(5) 0.0126(4) 0.0024(5) N1 0.0342(12) 0.0336(12) 0.0359(12) 0.0034(10) 0.0092(9) 0.0068(9) N2 0.0295(11) 0.0344(12) 0.0308(11) 0.0034(9) 0.0045(9) 0.0008(9) N3 0.0297(11) 0.0304(12) 0.0291(11) 0.0010(9) 0.0053(9) 0.0012(9) N4 0.0331(11) 0.0305(12) 0.0330(12) 0.0022(9) 0.0068(9) 0.0030(9) N5 0.0544(16) 0.0558(16) 0.0349(13) 0.0027(12) 0.0147(12) 0.0145(12) N6 0.0415(14) 0.0698(18) 0.0308(13) 0.0057(12) 0.0076(11) -0.0070(12) C1 0.0470(16) 0.0294(15) 0.0378(15) 0.0022(11) 0.0035(13) 0.0061(12) C2 0.0585(19) 0.0344(16) 0.0438(17) 0.0045(13) -0.0020(14) 0.0084(14) C3 0.076(2) 0.0308(17) 0.057(2) 0.0075(15) 0.0018(17) 0.0024(15) C4 0.090(3) 0.039(2) 0.069(2) -0.0025(17) 0.004(2) -0.0093(18) C5 0.066(2) 0.049(2) 0.060(2) -0.0089(17) -0.0042(18) -0.0026(17) C6 0.062(2) 0.0421(18) 0.0425(17) -0.0059(14) 0.0025(15) 0.0069(15) C7 0.0418(15) 0.0324(15) 0.0402(15) 0.0016(12) 0.0082(12) 0.0107(12) C8 0.0546(19) 0.0424(17) 0.0441(17) -0.0042(13) 0.0158(14) 0.0109(14) C9 0.0416(16) 0.0498(18) 0.0476(18) 0.0044(14) 0.0198(14) 0.0122(13) C10 0.0318(14) 0.0395(16) 0.0405(15) 0.0070(12) 0.0097(12) 0.0107(11) C11 0.0294(13) 0.0460(17) 0.0361(15) 0.0096(12) 0.0069(11) 0.0054(11) C12 0.0351(15) 0.063(2) 0.0439(17) 0.0147(15) 0.0105(13) 0.0018(14) C13 0.0414(18) 0.082(3) 0.061(2) 0.0036(19) 0.0107(16) -0.0143(17) C14 0.0339(17) 0.126(4) 0.057(2) 0.011(2) -0.0009(16) -0.006(2) C15 0.0391(18) 0.101(3) 0.049(2) 0.022(2) -0.0024(15) 0.0135(18) C16 0.0367(16) 0.062(2) 0.0525(19) 0.0213(16) 0.0090(14) 0.0132(14) C17 0.0269(13) 0.0372(15) 0.0350(14) 0.0050(11) 0.0040(11) -0.0003(10) C18 0.0345(14) 0.0474(17) 0.0323(14) 0.0060(12) 0.0015(11) -0.0010(12) C19 0.0383(15) 0.0417(16) 0.0347(15) -0.0029(12) 0.0079(12) -0.0018(12) C20 0.0318(13) 0.0330(14) 0.0355(14) 0.0001(11) 0.0073(11) -0.0018(11) C21 0.0327(13) 0.0287(14) 0.0374(14) 0.0012(11) 0.0063(11) -0.0001(10) C22 0.0429(16) 0.0340(15) 0.0463(17) 0.0050(13) 0.0091(13) -0.0033(12) C23 0.056(2) 0.048(2) 0.065(2) -0.0004(16) 0.0071(17) -0.0158(16) C24 0.080(3) 0.0395(19) 0.071(2) -0.0140(17) 0.011(2) -0.0107(17) C25 0.066(2) 0.0429(19) 0.053(2) -0.0067(15) 0.0140(16) 0.0085(15) C26 0.0416(16) 0.0360(16) 0.0511(18) -0.0002(13) 0.0121(14) 0.0029(12) C27 0.0303(13) 0.0280(13) 0.0353(14) 0.0022(11) 0.0059(11) 0.0025(10) C28 0.0369(14) 0.0330(15) 0.0392(15) 0.0082(12) 0.0074(12) 0.0020(11) C29 0.0362(14) 0.0408(16) 0.0307(14) 0.0026(12) 0.0026(11) 0.0050(12) C30 0.0276(12) 0.0331(14) 0.0323(14) 0.0017(11) 0.0044(10) 0.0030(10) C31 0.0302(13) 0.0336(14) 0.0333(14) -0.0011(11) 0.0048(11) 0.0008(10) C32 0.0314(14) 0.0461(17) 0.0449(17) -0.0014(13) 0.0080(12) 0.0021(12) C33 0.0416(17) 0.058(2) 0.061(2) 0.0100(17) 0.0107(15) 0.0166(15) C34 0.0389(18) 0.088(3) 0.060(2) 0.011(2) -0.0054(16) 0.0058(17) C35 0.0487(19) 0.069(2) 0.0435(18) -0.0007(16) -0.0063(15) -0.0083(16) C36 0.0393(16) 0.0464(18) 0.0441(17) -0.0048(14) 0.0025(13) -0.0043(13) C37 0.0293(13) 0.0328(14) 0.0353(14) -0.0009(11) 0.0052(11) -0.0008(10) C38 0.0402(15) 0.0392(16) 0.0397(15) 0.0004(12) 0.0138(12) -0.0020(12) C39 0.0506(17) 0.0332(15) 0.0413(16) 0.0069(12) 0.0108(13) -0.0020(12) C40 0.0394(14) 0.0275(14) 0.0359(14) -0.0008(11) 0.0052(11) -0.0014(11) C41 0.112(4) 0.078(3) 0.074(3) -0.016(2) 0.035(3) -0.019(3) C42 0.109(4) 0.105(4) 0.043(2) 0.002(2) -0.004(2) -0.004(3) C43 0.114(4) 0.100(4) 0.095(4) -0.037(3) 0.020(3) 0.038(3) C44 0.089(3) 0.084(3) 0.069(3) 0.027(2) 0.003(2) -0.007(2) C45 0.070(3) 0.144(5) 0.082(3) -0.024(3) 0.040(2) -0.001(3) C46 0.075(3) 0.101(3) 0.057(2) -0.003(2) 0.008(2) 0.002(2) C47 0.071(3) 0.078(3) 0.062(2) 0.008(2) 0.017(2) 0.005(2) C48 0.082(3) 0.155(5) 0.128(4) 0.073(4) 0.067(3) 0.032(3) C49 0.133(5) 0.145(5) 0.072(3) -0.046(3) 0.000(3) 0.022(4) C50 0.078(3) 0.138(5) 0.167(5) 0.103(4) 0.017(3) -0.012(3) C51 0.079(3) 0.061(2) 0.066(2) 0.0118(19) 0.026(2) 0.004(2) C52 0.132(5) 0.237(8) 0.039(2) -0.009(3) -0.008(3) 0.096(5) C53 0.31(2) 0.35(3) 0.29(2) -0.02(2) -0.01(2) 0.01(3) C54 0.49(4) 0.37(3) 0.34(3) -0.15(2) -0.12(3) 0.05(3) C55 0.36(3) 0.222(16) 0.58(4) 0.03(2) -0.16(3) -0.069(17) _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 Nd2 N6 2.321(2) . ? Nd2 N1 2.676(2) . ? Nd2 N3 2.715(2) . ? Nd2 N4 2.746(2) . ? Nd2 N2 2.778(2) . ? Nd2 C40 2.854(3) . ? Nd2 C20 2.858(3) . ? Nd2 C37 2.872(3) . ? Nd2 C17 2.887(2) . ? Nd2 C19 2.902(3) . ? Nd2 C18 2.915(3) . ? Nd2 C39 2.942(3) . ? Nd2 C38 2.953(3) . ? Nd2 Nd1 3.4827(2) . ? Nd1 N5 2.325(2) . ? Nd1 N4 2.694(2) . ? Nd1 N2 2.736(2) . ? Nd1 N1 2.751(2) . ? Nd1 N3 2.756(2) . ? Nd1 C30 2.852(2) . ? Nd1 C10 2.854(3) . ? Nd1 C27 2.871(3) . ? Nd1 C7 2.877(3) . ? Nd1 C29 2.911(3) . ? Nd1 C28 2.924(3) . ? Nd1 C9 2.943(3) . ? Nd1 C8 2.958(3) . ? Si1 N5 1.715(3) . ? Si1 C42 1.860(4) . ? Si1 C41 1.868(4) . ? Si1 C43 1.869(4) . ? Si2 N5 1.711(3) . ? Si2 C45 1.870(4) . ? Si2 C46 1.871(4) . ? Si2 C44 1.880(4) . ? Si3 N6 1.708(3) . ? Si3 C49 1.867(5) . ? Si3 C48 1.868(4) . ? Si3 C47 1.869(4) . ? Si4 N6 1.714(3) . ? Si4 C52 1.850(4) . ? Si4 C51 1.853(4) . ? Si4 C50 1.884(5) . ? N1 C7 1.382(4) . ? N1 C10 1.391(3) . ? N2 C17 1.384(3) . ? N2 C20 1.385(3) . ? N3 C27 1.383(3) . ? N3 C30 1.387(3) . ? N4 C37 1.386(3) . ? N4 C40 1.387(3) . ? C1 C7 1.500(4) . ? C1 C40 1.512(4) . ? C1 C6 1.540(4) . ? C1 C2 1.549(4) . ? C2 C3 1.521(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.517(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.519(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.519(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.383(4) . ? C8 C9 1.420(4) . ? C8 H8 0.9300 . ? C9 C10 1.385(4) . ? C9 H9 0.9300 . ? C10 C11 1.488(4) . ? C11 C17 1.514(4) . ? C11 C16 1.541(4) . ? C11 C12 1.546(4) . ? C12 C13 1.515(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.513(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.525(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.518(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.377(4) . ? C18 C19 1.421(4) . ? C18 H18 0.9300 . ? C19 C20 1.377(4) . ? C19 H19 0.9300 . ? C20 C21 1.507(4) . ? C21 C27 1.505(4) . ? C21 C22 1.542(4) . ? C21 C26 1.551(4) . ? C22 C23 1.517(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.520(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.521(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.522(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.370(4) . ? C28 C29 1.421(4) . ? C28 H28 0.9300 . ? C29 C30 1.379(4) . ? C29 H29 0.9300 . ? C30 C31 1.510(3) . ? C31 C37 1.499(4) . ? C31 C32 1.540(4) . ? C31 C36 1.543(4) . ? C32 C33 1.521(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.514(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.513(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.527(4) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.383(4) . ? C38 C39 1.420(4) . ? C38 H38 0.9300 . ? C39 C40 1.380(4) . ? C39 H39 0.9300 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.54(3) . ? C53 C53 1.56(5) 3_676 ? C54 C55 1.67(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 N6 Nd2 N1 126.53(8) . . ? N6 Nd2 N3 131.45(8) . . ? N1 Nd2 N3 102.02(6) . . ? N6 Nd2 N4 129.99(8) . . ? N1 Nd2 N4 66.35(7) . . ? N3 Nd2 N4 65.70(6) . . ? N6 Nd2 N2 130.14(8) . . ? N1 Nd2 N2 66.34(7) . . ? N3 Nd2 N2 65.99(6) . . ? N4 Nd2 N2 99.82(6) . . ? N6 Nd2 C40 109.11(9) . . ? N1 Nd2 C40 59.37(7) . . ? N3 Nd2 C40 94.18(7) . . ? N4 Nd2 C40 28.59(7) . . ? N2 Nd2 C40 115.95(7) . . ? N6 Nd2 C20 111.53(9) . . ? N1 Nd2 C20 94.67(7) . . ? N3 Nd2 C20 58.75(7) . . ? N4 Nd2 C20 115.17(7) . . ? N2 Nd2 C20 28.41(6) . . ? C40 Nd2 C20 139.35(7) . . ? N6 Nd2 C37 111.85(8) . . ? N1 Nd2 C37 94.76(7) . . ? N3 Nd2 C37 57.70(7) . . ? N4 Nd2 C37 28.45(6) . . ? N2 Nd2 C37 114.57(7) . . ? C40 Nd2 C37 45.41(7) . . ? C20 Nd2 C37 116.34(8) . . ? N6 Nd2 C17 110.14(8) . . ? N1 Nd2 C17 58.48(7) . . ? N3 Nd2 C17 94.15(7) . . ? N4 Nd2 C17 114.94(7) . . ? N2 Nd2 C17 28.20(6) . . ? C40 Nd2 C17 117.69(8) . . ? C20 Nd2 C17 45.23(7) . . ? C37 Nd2 C17 138.00(7) . . ? N6 Nd2 C19 85.51(9) . . ? N1 Nd2 C19 104.02(7) . . ? N3 Nd2 C19 82.74(7) . . ? N4 Nd2 C19 142.78(7) . . ? N2 Nd2 C19 46.92(7) . . ? C40 Nd2 C19 162.24(7) . . ? C20 Nd2 C19 27.64(7) . . ? C37 Nd2 C19 139.10(8) . . ? C17 Nd2 C19 45.58(8) . . ? N6 Nd2 C18 84.77(8) . . ? N1 Nd2 C18 81.80(7) . . ? N3 Nd2 C18 104.37(7) . . ? N4 Nd2 C18 142.38(7) . . ? N2 Nd2 C18 46.82(7) . . ? C40 Nd2 C18 139.82(8) . . ? C20 Nd2 C18 45.77(8) . . ? C37 Nd2 C18 160.82(8) . . ? C17 Nd2 C18 27.45(7) . . ? C19 Nd2 C18 28.28(8) . . ? N6 Nd2 C39 84.21(9) . . ? N1 Nd2 C39 83.39(7) . . ? N3 Nd2 C39 103.05(7) . . ? N4 Nd2 C39 46.87(7) . . ? N2 Nd2 C39 143.33(7) . . ? C40 Nd2 C39 27.49(7) . . ? C20 Nd2 C39 161.00(8) . . ? C37 Nd2 C39 45.39(8) . . ? C17 Nd2 C39 140.81(8) . . ? C19 Nd2 C39 169.61(8) . . ? C18 Nd2 C39 150.98(8) . . ? N6 Nd2 C38 85.82(8) . . ? N1 Nd2 C38 104.75(7) . . ? N3 Nd2 C38 81.19(7) . . ? N4 Nd2 C38 46.86(7) . . ? N2 Nd2 C38 142.00(7) . . ? C40 Nd2 C38 45.53(8) . . ? C20 Nd2 C38 138.45(8) . . ? C37 Nd2 C38 27.43(7) . . ? C17 Nd2 C38 161.49(8) . . ? C19 Nd2 C38 149.36(8) . . ? C18 Nd2 C38 170.53(8) . . ? C39 Nd2 C38 27.88(8) . . ? N6 Nd2 Nd1 177.51(7) . . ? N1 Nd2 Nd1 51.03(5) . . ? N3 Nd2 Nd1 51.00(4) . . ? N4 Nd2 Nd1 49.53(4) . . ? N2 Nd2 Nd1 50.29(4) . . ? C40 Nd2 Nd1 69.48(5) . . ? C20 Nd2 Nd1 69.88(5) . . ? C37 Nd2 Nd1 68.75(5) . . ? C17 Nd2 Nd1 69.26(5) . . ? C19 Nd2 Nd1 95.52(5) . . ? C18 Nd2 Nd1 95.06(5) . . ? C39 Nd2 Nd1 94.81(6) . . ? C38 Nd2 Nd1 94.39(5) . . ? N5 Nd1 N4 126.86(9) . . ? N5 Nd1 N2 130.90(8) . . ? N4 Nd1 N2 102.23(6) . . ? N5 Nd1 N1 130.86(7) . . ? N4 Nd1 N1 66.04(6) . . ? N2 Nd1 N1 65.93(7) . . ? N5 Nd1 N3 130.00(7) . . ? N4 Nd1 N3 65.84(6) . . ? N2 Nd1 N3 66.02(6) . . ? N1 Nd1 N3 99.07(6) . . ? N5 Nd1 C30 109.20(8) . . ? N4 Nd1 C30 58.89(7) . . ? N2 Nd1 C30 94.46(7) . . ? N1 Nd1 C30 115.17(7) . . ? N3 Nd1 C30 28.57(7) . . ? N5 Nd1 C10 111.94(8) . . ? N4 Nd1 C10 94.64(7) . . ? N2 Nd1 C10 58.39(7) . . ? N1 Nd1 C10 28.68(7) . . ? N3 Nd1 C10 114.73(7) . . ? C30 Nd1 C10 138.86(7) . . ? N5 Nd1 C27 111.94(8) . . ? N4 Nd1 C27 94.18(7) . . ? N2 Nd1 C27 57.74(7) . . ? N1 Nd1 C27 113.87(7) . . ? N3 Nd1 C27 28.37(6) . . ? C30 Nd1 C27 45.40(7) . . ? C10 Nd1 C27 115.96(8) . . ? N5 Nd1 C7 110.76(8) . . ? N4 Nd1 C7 58.22(7) . . ? N2 Nd1 C7 94.20(7) . . ? N1 Nd1 C7 28.32(7) . . ? N3 Nd1 C7 114.22(7) . . ? C30 Nd1 C7 116.95(8) . . ? C10 Nd1 C7 45.53(8) . . ? C27 Nd1 C7 137.29(7) . . ? N5 Nd1 C29 84.11(8) . . ? N4 Nd1 C29 83.12(7) . . ? N2 Nd1 C29 103.21(7) . . ? N1 Nd1 C29 142.71(7) . . ? N3 Nd1 C29 46.99(7) . . ? C30 Nd1 C29 27.66(7) . . ? C10 Nd1 C29 160.69(8) . . ? C27 Nd1 C29 45.50(8) . . ? C7 Nd1 C29 140.31(8) . . ? N5 Nd1 C28 85.90(8) . . ? N4 Nd1 C28 104.51(7) . . ? N2 Nd1 C28 80.84(7) . . ? N1 Nd1 C28 141.20(7) . . ? N3 Nd1 C28 46.88(7) . . ? C30 Nd1 C28 45.81(7) . . ? C10 Nd1 C28 137.91(8) . . ? C27 Nd1 C28 27.33(7) . . ? C7 Nd1 C28 160.84(7) . . ? C29 Nd1 C28 28.20(8) . . ? N5 Nd1 C9 86.18(8) . . ? N4 Nd1 C9 103.59(8) . . ? N2 Nd1 C9 82.49(8) . . ? N1 Nd1 C9 46.86(7) . . ? N3 Nd1 C9 142.24(7) . . ? C30 Nd1 C9 161.32(8) . . ? C10 Nd1 C9 27.60(8) . . ? C27 Nd1 C9 139.19(8) . . ? C7 Nd1 C9 45.42(8) . . ? C29 Nd1 C9 170.24(8) . . ? C28 Nd1 C9 149.74(8) . . ? N5 Nd1 C8 85.61(8) . . ? N4 Nd1 C8 81.72(7) . . ? N2 Nd1 C8 103.85(8) . . ? N1 Nd1 C8 46.67(7) . . ? N3 Nd1 C8 141.58(7) . . ? C30 Nd1 C8 139.39(8) . . ? C10 Nd1 C8 45.59(9) . . ? C27 Nd1 C8 160.04(8) . . ? C7 Nd1 C8 27.38(7) . . ? C29 Nd1 C8 151.20(9) . . ? C28 Nd1 C8 171.41(8) . . ? C9 Nd1 C8 27.85(9) . . ? N5 Nd1 Nd2 177.72(7) . . ? N4 Nd1 Nd2 50.86(5) . . ? N2 Nd1 Nd2 51.38(4) . . ? N1 Nd1 Nd2 49.13(4) . . ? N3 Nd1 Nd2 49.94(4) . . ? C30 Nd1 Nd2 69.85(5) . . ? C10 Nd1 Nd2 69.02(5) . . ? C27 Nd1 Nd2 68.98(5) . . ? C7 Nd1 Nd2 68.30(5) . . ? C29 Nd1 Nd2 95.36(5) . . ? C28 Nd1 Nd2 94.68(5) . . ? C9 Nd1 Nd2 94.38(6) . . ? C8 Nd1 Nd2 93.85(6) . . ? N5 Si1 C42 113.96(18) . . ? N5 Si1 C41 109.36(16) . . ? C42 Si1 C41 104.8(2) . . ? N5 Si1 C43 114.26(19) . . ? C42 Si1 C43 106.7(2) . . ? C41 Si1 C43 107.1(2) . . ? N5 Si2 C45 113.5(2) . . ? N5 Si2 C46 109.46(16) . . ? C45 Si2 C46 106.2(2) . . ? N5 Si2 C44 114.20(17) . . ? C45 Si2 C44 107.4(2) . . ? C46 Si2 C44 105.5(2) . . ? N6 Si3 C49 113.8(2) . . ? N6 Si3 C48 114.1(2) . . ? C49 Si3 C48 106.4(3) . . ? N6 Si3 C47 108.56(15) . . ? C49 Si3 C47 106.4(2) . . ? C48 Si3 C47 107.1(2) . . ? N6 Si4 C52 114.8(2) . . ? N6 Si4 C51 109.88(15) . . ? C52 Si4 C51 105.5(2) . . ? N6 Si4 C50 113.64(18) . . ? C52 Si4 C50 106.3(3) . . ? C51 Si4 C50 106.0(2) . . ? C7 N1 C10 106.2(2) . . ? C7 N1 Nd2 122.08(16) . . ? C10 N1 Nd2 123.04(17) . . ? C7 N1 Nd1 80.94(15) . . ? C10 N1 Nd1 79.77(14) . . ? Nd2 N1 Nd1 79.84(6) . . ? C17 N2 C20 105.8(2) . . ? C17 N2 Nd1 121.36(17) . . ? C20 N2 Nd1 122.25(16) . . ? C17 N2 Nd2 80.24(14) . . ? C20 N2 Nd2 78.97(14) . . ? Nd1 N2 Nd2 78.33(6) . . ? C27 N3 C30 105.7(2) . . ? C27 N3 Nd2 121.42(16) . . ? C30 N3 Nd2 123.21(16) . . ? C27 N3 Nd1 80.41(13) . . ? C30 N3 Nd1 79.55(13) . . ? Nd2 N3 Nd1 79.06(5) . . ? C37 N4 C40 105.7(2) . . ? C37 N4 Nd1 121.95(16) . . ? C40 N4 Nd1 123.53(16) . . ? C37 N4 Nd2 80.82(14) . . ? C40 N4 Nd2 80.02(15) . . ? Nd1 N4 Nd2 79.61(6) . . ? Si2 N5 Si1 119.63(14) . . ? Si2 N5 Nd1 119.66(14) . . ? Si1 N5 Nd1 120.71(14) . . ? Si3 N6 Si4 121.22(14) . . ? Si3 N6 Nd2 118.98(14) . . ? Si4 N6 Nd2 119.79(14) . . ? C7 C1 C40 104.5(2) . . ? C7 C1 C6 111.9(2) . . ? C40 C1 C6 109.9(2) . . ? C7 C1 C2 108.3(2) . . ? C40 C1 C2 114.5(2) . . ? C6 C1 C2 107.8(2) . . ? C3 C2 C1 114.9(3) . . ? C3 C2 H2A 108.6 . . ? C1 C2 H2A 108.6 . . ? C3 C2 H2B 108.6 . . ? C1 C2 H2B 108.6 . . ? H2A C2 H2B 107.5 . . ? C4 C3 C2 112.0(3) . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C3 C4 C5 110.3(3) . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4B 109.6 . . ? C5 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C6 C5 C4 111.0(3) . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C1 112.3(3) . . ? C5 C6 H6A 109.2 . . ? C1 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C1 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N1 C7 C8 110.3(3) . . ? N1 C7 C1 117.0(2) . . ? C8 C7 C1 132.5(3) . . ? N1 C7 Nd1 70.74(14) . . ? C8 C7 Nd1 79.54(17) . . ? C1 C7 Nd1 119.91(17) . . ? C7 C8 C9 106.6(3) . . ? C7 C8 Nd1 73.08(16) . . ? C9 C8 Nd1 75.50(17) . . ? C7 C8 H8 126.7 . . ? C9 C8 H8 126.7 . . ? Nd1 C8 H8 116.9 . . ? C10 C9 C8 106.9(3) . . ? C10 C9 Nd1 72.61(16) . . ? C8 C9 Nd1 76.66(16) . . ? C10 C9 H9 126.6 . . ? C8 C9 H9 126.6 . . ? Nd1 C9 H9 116.4 . . ? C9 C10 N1 109.7(3) . . ? C9 C10 C11 133.0(3) . . ? N1 C10 C11 116.8(2) . . ? C9 C10 Nd1 79.79(17) . . ? N1 C10 Nd1 71.55(14) . . ? C11 C10 Nd1 120.13(17) . . ? C10 C11 C17 104.5(2) . . ? C10 C11 C16 108.4(2) . . ? C17 C11 C16 115.2(2) . . ? C10 C11 C12 112.3(2) . . ? C17 C11 C12 108.9(2) . . ? C16 C11 C12 107.6(2) . . ? C13 C12 C11 112.5(2) . . ? C13 C12 H12A 109.1 . . ? C11 C12 H12A 109.1 . . ? C13 C12 H12B 109.1 . . ? C11 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C14 C13 C12 111.3(3) . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C13 C14 C15 110.8(3) . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C14 111.4(3) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C11 115.3(3) . . ? C15 C16 H16A 108.5 . . ? C11 C16 H16A 108.5 . . ? C15 C16 H16B 108.5 . . ? C11 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? C18 C17 N2 110.3(2) . . ? C18 C17 C11 135.0(2) . . ? N2 C17 C11 114.6(2) . . ? C18 C17 Nd2 77.44(15) . . ? N2 C17 Nd2 71.56(13) . . ? C11 C17 Nd2 119.64(18) . . ? C17 C18 C19 106.5(2) . . ? C17 C18 Nd2 75.11(16) . . ? C19 C18 Nd2 75.33(16) . . ? C17 C18 H18 126.7 . . ? C19 C18 H18 126.7 . . ? Nd2 C18 H18 115.2 . . ? C20 C19 C18 106.8(2) . . ? C20 C19 Nd2 74.40(16) . . ? C18 C19 Nd2 76.40(16) . . ? C20 C19 H19 126.6 . . ? C18 C19 H19 126.6 . . ? Nd2 C19 H19 115.0 . . ? C19 C20 N2 110.1(2) . . ? C19 C20 C21 134.9(3) . . ? N2 C20 C21 114.7(2) . . ? C19 C20 Nd2 77.96(16) . . ? N2 C20 Nd2 72.61(14) . . ? C21 C20 Nd2 119.75(16) . . ? C27 C21 C20 104.3(2) . . ? C27 C21 C22 112.7(2) . . ? C20 C21 C22 109.5(2) . . ? C27 C21 C26 107.4(2) . . ? C20 C21 C26 115.1(2) . . ? C22 C21 C26 107.9(2) . . ? C23 C22 C21 112.9(2) . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22B 109.0 . . ? C21 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C22 C23 C24 111.8(3) . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? C23 C24 C25 110.4(3) . . ? C23 C24 H24A 109.6 . . ? C25 C24 H24A 109.6 . . ? C23 C24 H24B 109.6 . . ? C25 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C24 C25 C26 111.3(3) . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C21 114.7(2) . . ? C25 C26 H26A 108.6 . . ? C21 C26 H26A 108.6 . . ? C25 C26 H26B 108.6 . . ? C21 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C28 C27 N3 110.7(2) . . ? C28 C27 C21 133.3(2) . . ? N3 C27 C21 115.7(2) . . ? C28 C27 Nd1 78.48(16) . . ? N3 C27 Nd1 71.22(13) . . ? C21 C27 Nd1 121.15(16) . . ? C27 C28 C29 106.4(2) . . ? C27 C28 Nd1 74.19(15) . . ? C29 C28 Nd1 75.40(15) . . ? C27 C28 H28 126.8 . . ? C29 C28 H28 126.8 . . ? Nd1 C28 H28 116.0 . . ? C30 C29 C28 106.8(2) . . ? C30 C29 Nd1 73.80(15) . . ? C28 C29 Nd1 76.39(15) . . ? C30 C29 H29 126.6 . . ? C28 C29 H29 126.6 . . ? Nd1 C29 H29 115.6 . . ? C29 C30 N3 109.9(2) . . ? C29 C30 C31 135.4(2) . . ? N3 C30 C31 114.4(2) . . ? C29 C30 Nd1 78.53(15) . . ? N3 C30 Nd1 71.88(13) . . ? C31 C30 Nd1 119.72(16) . . ? C37 C31 C30 104.3(2) . . ? C37 C31 C32 113.4(2) . . ? C30 C31 C32 108.9(2) . . ? C37 C31 C36 106.5(2) . . ? C30 C31 C36 116.0(2) . . ? C32 C31 C36 107.9(2) . . ? C33 C32 C31 112.3(2) . . ? C33 C32 H32A 109.1 . . ? C31 C32 H32A 109.1 . . ? C33 C32 H32B 109.1 . . ? C31 C32 H32B 109.1 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C32 111.7(3) . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33B 109.3 . . ? C32 C33 H33B 109.3 . . ? H33A C33 H33B 107.9 . . ? C35 C34 C33 110.9(3) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 111.4(3) . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? C34 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C31 115.1(3) . . ? C35 C36 H36A 108.5 . . ? C31 C36 H36A 108.5 . . ? C35 C36 H36B 108.5 . . ? C31 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? C38 C37 N4 110.4(2) . . ? C38 C37 C31 133.0(2) . . ? N4 C37 C31 116.2(2) . . ? C38 C37 Nd2 79.55(16) . . ? N4 C37 Nd2 70.73(14) . . ? C31 C37 Nd2 120.94(17) . . ? C37 C38 C39 106.4(2) . . ? C37 C38 Nd2 73.02(16) . . ? C39 C38 Nd2 75.65(16) . . ? C37 C38 H38 126.8 . . ? C39 C38 H38 126.8 . . ? Nd2 C38 H38 116.8 . . ? C40 C39 C38 106.9(2) . . ? C40 C39 Nd2 72.68(16) . . ? C38 C39 Nd2 76.47(16) . . ? C40 C39 H39 126.6 . . ? C38 C39 H39 126.6 . . ? Nd2 C39 H39 116.5 . . ? C39 C40 N4 110.2(2) . . ? C39 C40 C1 134.3(3) . . ? N4 C40 C1 115.2(2) . . ? C39 C40 Nd2 79.83(17) . . ? N4 C40 Nd2 71.39(14) . . ? C1 C40 Nd2 118.92(18) . . ? Si1 C41 H41A 109.5 . . ? Si1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si1 C42 H42A 109.5 . . ? Si1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si2 C44 H44A 109.5 . . ? Si2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si2 C45 H45A 109.5 . . ? Si2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si2 C46 H46A 109.5 . . ? Si2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? Si3 C47 H47A 109.5 . . ? Si3 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si3 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Si3 C48 H48A 109.5 . . ? Si3 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si3 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Si3 C49 H49A 109.5 . . ? Si3 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? Si3 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? Si4 C50 H50A 109.5 . . ? Si4 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Si4 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Si4 C51 H51A 109.5 . . ? Si4 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si4 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si4 C52 H52A 109.5 . . ? Si4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C53 92(3) . 3_676 ? C53 C54 C55 69.1(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.589 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.079 # Attachment '4907_web_deposit_cif_file_4_ShuangliuZhou_1301667625.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 819831' #TrackingRef '4907_web_deposit_cif_file_4_ShuangliuZhou_1301667625.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H84 N6 Si4 Sm2' _chemical_formula_weight 1242.34 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 12.6353(10) _cell_length_b 29.185(2) _cell_length_c 19.4542(11) _cell_angle_alpha 90.00 _cell_angle_beta 122.871(4) _cell_angle_gamma 90.00 _cell_volume 6025.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 2.048 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6733 _exptl_absorpt_correction_T_max 0.709 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46785 _diffrn_reflns_av_R_equivalents 0.1494 _diffrn_reflns_av_sigmaI/netI 0.1487 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11805 _reflns_number_gt 6227 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+0.2144P] 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 11805 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1467 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1164 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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 Sm1 Sm 0.35226(4) 0.352930(14) 0.23708(3) 0.03211(13) Uani 1 1 d . . . Sm2 Sm 0.60874(4) 0.362728(14) 0.43534(3) 0.03380(13) Uani 1 1 d . . . Si1 Si 0.0587(2) 0.37971(10) 0.06647(18) 0.0612(8) Uani 1 1 d . . . Si2 Si 0.1859(3) 0.30053(11) 0.04486(18) 0.0645(9) Uani 1 1 d . . . Si3 Si 0.7896(3) 0.33009(10) 0.64170(17) 0.0580(8) Uani 1 1 d . . . Si4 Si 0.8909(2) 0.40754(10) 0.59713(17) 0.0581(8) Uani 1 1 d . . . N5 N 0.1848(6) 0.3437(2) 0.1042(4) 0.0444(19) Uani 1 1 d . . . N6 N 0.7777(6) 0.3670(2) 0.5692(4) 0.0442(19) Uani 1 1 d . . . N1 N 0.4041(6) 0.3104(2) 0.3769(4) 0.0312(16) Uani 1 1 d . . . N2 N 0.5668(6) 0.3061(2) 0.3115(4) 0.0338(17) Uani 1 1 d . . . N3 N 0.5622(6) 0.4067(2) 0.2992(4) 0.0329(17) Uani 1 1 d . . . N4 N 0.3877(6) 0.4108(2) 0.3559(4) 0.0312(16) Uani 1 1 d . . . C10 C 0.3786(8) 0.2725(3) 0.3267(5) 0.036(2) Uani 1 1 d . . . C9 C 0.2516(8) 0.2709(3) 0.2673(5) 0.045(2) Uani 1 1 d . . . H9 H 0.2123 0.2499 0.2247 0.054 Uiso 1 1 calc R . . C8 C 0.1919(8) 0.3065(3) 0.2822(5) 0.043(2) Uani 1 1 d . . . H8 H 0.1065 0.3136 0.2520 0.051 Uiso 1 1 calc R . . C7 C 0.2865(8) 0.3286(3) 0.3511(5) 0.035(2) Uani 1 1 d . . . C1 C 0.2866(7) 0.3640(3) 0.4078(5) 0.038(2) Uani 1 1 d . . . C2 C 0.1613(7) 0.3910(3) 0.3684(5) 0.040(2) Uani 1 1 d . . . H2A H 0.1525 0.4102 0.3249 0.048 Uiso 1 1 calc R . . H2B H 0.0913 0.3696 0.3444 0.048 Uiso 1 1 calc R . . C3 C 0.1565(8) 0.4208(3) 0.4310(6) 0.054(3) Uani 1 1 d . . . H3A H 0.2232 0.4435 0.4522 0.065 Uiso 1 1 calc R . . H3B H 0.0767 0.4370 0.4040 0.065 Uiso 1 1 calc R . . C4 C 0.1707(9) 0.3936(3) 0.5010(6) 0.065(3) Uani 1 1 d . . . H4A H 0.0994 0.3731 0.4810 0.078 Uiso 1 1 calc R . . H4B H 0.1716 0.4142 0.5404 0.078 Uiso 1 1 calc R . . C5 C 0.2908(8) 0.3663(3) 0.5420(6) 0.055(3) Uani 1 1 d . . . H5A H 0.2934 0.3464 0.5828 0.066 Uiso 1 1 calc R . . H5B H 0.3620 0.3870 0.5699 0.066 Uiso 1 1 calc R . . C6 C 0.3023(8) 0.3375(3) 0.4813(5) 0.040(2) Uani 1 1 d . . . H6A H 0.2393 0.3134 0.4607 0.048 Uiso 1 1 calc R . . H6B H 0.3844 0.3228 0.5101 0.048 Uiso 1 1 calc R . . C40 C 0.3909(7) 0.3965(2) 0.4253(5) 0.0280(19) Uani 1 1 d . . . C39 C 0.4839(7) 0.4194(3) 0.4924(5) 0.040(2) Uani 1 1 d . . . H39 H 0.5078 0.4144 0.5462 0.048 Uiso 1 1 calc R . . C38 C 0.5376(7) 0.4519(3) 0.4663(5) 0.036(2) Uani 1 1 d . . . H38 H 0.6033 0.4721 0.4986 0.043 Uiso 1 1 calc R . . C37 C 0.4717(7) 0.4471(3) 0.3827(5) 0.030(2) Uani 1 1 d . . . C31 C 0.4662(7) 0.4747(3) 0.3155(5) 0.035(2) Uani 1 1 d . . . C32 C 0.3428(7) 0.5037(3) 0.2756(5) 0.041(2) Uani 1 1 d . . . H32A H 0.2713 0.4830 0.2507 0.049 Uiso 1 1 calc R . . H32B H 0.3421 0.5205 0.3184 0.049 Uiso 1 1 calc R . . C33 C 0.3258(8) 0.5381(3) 0.2101(6) 0.055(3) Uani 1 1 d . . . H33A H 0.3140 0.5216 0.1631 0.066 Uiso 1 1 calc R . . H33B H 0.2515 0.5567 0.1920 0.066 Uiso 1 1 calc R . . C34 C 0.4410(8) 0.5689(3) 0.2451(6) 0.063(3) Uani 1 1 d . . . H34A H 0.4472 0.5879 0.2880 0.075 Uiso 1 1 calc R . . H34B H 0.4319 0.5890 0.2024 0.075 Uiso 1 1 calc R . . C35 C 0.5609(8) 0.5405(3) 0.2797(6) 0.055(3) Uani 1 1 d . . . H35A H 0.5572 0.5229 0.2361 0.066 Uiso 1 1 calc R . . H35B H 0.6334 0.5607 0.3028 0.066 Uiso 1 1 calc R . . C36 C 0.5756(7) 0.5082(3) 0.3455(5) 0.040(2) Uani 1 1 d . . . H36A H 0.5836 0.5262 0.3900 0.048 Uiso 1 1 calc R . . H36B H 0.6528 0.4908 0.3670 0.048 Uiso 1 1 calc R . . C30 C 0.4683(7) 0.4396(3) 0.2590(5) 0.035(2) Uani 1 1 d . . . C29 C 0.4062(7) 0.4337(3) 0.1762(5) 0.038(2) Uani 1 1 d . . . H29 H 0.3360 0.4499 0.1364 0.046 Uiso 1 1 calc R . . C28 C 0.4689(7) 0.3982(3) 0.1626(5) 0.039(2) Uani 1 1 d . . . H28 H 0.4470 0.3863 0.1122 0.046 Uiso 1 1 calc R . . C27 C 0.5689(7) 0.3845(3) 0.2385(5) 0.033(2) Uani 1 1 d . . . C21 C 0.6807(7) 0.3537(3) 0.2697(5) 0.037(2) Uani 1 1 d . . . C26 C 0.8005(7) 0.3833(3) 0.3050(5) 0.047(2) Uani 1 1 d . . . H26A H 0.8024 0.4055 0.3428 0.057 Uiso 1 1 calc R . . H26B H 0.8741 0.3638 0.3356 0.057 Uiso 1 1 calc R . . C25 C 0.8065(8) 0.4083(3) 0.2389(6) 0.066(3) Uani 1 1 d . . . H25A H 0.7345 0.4286 0.2096 0.079 Uiso 1 1 calc R . . H25B H 0.8822 0.4268 0.2641 0.079 Uiso 1 1 calc R . . C24 C 0.8068(10) 0.3754(4) 0.1793(7) 0.078(3) Uani 1 1 d . . . H24A H 0.8827 0.3569 0.2074 0.094 Uiso 1 1 calc R . . H24B H 0.8065 0.3925 0.1364 0.094 Uiso 1 1 calc R . . C23 C 0.6898(8) 0.3439(3) 0.1412(6) 0.060(3) Uani 1 1 d . . . H23A H 0.6148 0.3619 0.1057 0.071 Uiso 1 1 calc R . . H23B H 0.6963 0.3207 0.1080 0.071 Uiso 1 1 calc R . . C22 C 0.6778(8) 0.3211(3) 0.2061(5) 0.051(3) Uani 1 1 d . . . H22A H 0.7459 0.2991 0.2349 0.061 Uiso 1 1 calc R . . H22B H 0.5993 0.3041 0.1793 0.061 Uiso 1 1 calc R . . C20 C 0.6823(7) 0.3248(3) 0.3342(5) 0.034(2) Uani 1 1 d . . . C19 C 0.7761(7) 0.3081(3) 0.4081(5) 0.047(3) Uani 1 1 d . . . H19 H 0.8604 0.3169 0.4369 0.057 Uiso 1 1 calc R . . C18 C 0.7217(8) 0.2749(3) 0.4329(6) 0.048(2) Uani 1 1 d . . . H18 H 0.7624 0.2575 0.4806 0.057 Uiso 1 1 calc R . . C17 C 0.5957(8) 0.2737(3) 0.3713(6) 0.039(2) Uani 1 1 d . . . C11 C 0.4905(8) 0.2414(3) 0.3542(5) 0.039(2) Uani 1 1 d . . . C12 C 0.4703(8) 0.2064(3) 0.2881(5) 0.047(2) Uani 1 1 d . . . H12A H 0.4408 0.2229 0.2374 0.056 Uiso 1 1 calc R . . H12B H 0.5511 0.1929 0.3050 0.056 Uiso 1 1 calc R . . C13 C 0.3775(9) 0.1679(3) 0.2709(6) 0.061(3) Uani 1 1 d . . . H13A H 0.2930 0.1803 0.2448 0.074 Uiso 1 1 calc R . . H13B H 0.3784 0.1458 0.2340 0.074 Uiso 1 1 calc R . . C14 C 0.4128(10) 0.1447(3) 0.3492(6) 0.066(3) Uani 1 1 d . . . H14A H 0.4929 0.1291 0.3716 0.079 Uiso 1 1 calc R . . H14B H 0.3498 0.1218 0.3381 0.079 Uiso 1 1 calc R . . C15 C 0.4232(9) 0.1784(3) 0.4121(6) 0.061(3) Uani 1 1 d . . . H15A H 0.3420 0.1927 0.3915 0.074 Uiso 1 1 calc R . . H15B H 0.4477 0.1623 0.4622 0.074 Uiso 1 1 calc R . . C16 C 0.5196(8) 0.2147(3) 0.4295(5) 0.051(3) Uani 1 1 d . . . H16A H 0.6014 0.2002 0.4534 0.061 Uiso 1 1 calc R . . H16B H 0.5247 0.2359 0.4696 0.061 Uiso 1 1 calc R . . C41 C -0.0966(9) 0.3499(4) 0.0170(7) 0.122(5) Uani 1 1 d . . . H41A H -0.1158 0.3362 -0.0334 0.183 Uiso 1 1 calc R . . H41B H -0.1610 0.3717 0.0058 0.183 Uiso 1 1 calc R . . H41C H -0.0930 0.3266 0.0529 0.183 Uiso 1 1 calc R . . C42 C 0.0767(9) 0.4152(3) 0.1516(6) 0.069(3) Uani 1 1 d . . . H42A H 0.0609 0.3966 0.1858 0.104 Uiso 1 1 calc R . . H42B H 0.0176 0.4400 0.1295 0.104 Uiso 1 1 calc R . . H42C H 0.1608 0.4271 0.1833 0.104 Uiso 1 1 calc R . . C43 C 0.0455(12) 0.4202(4) -0.0116(7) 0.127(5) Uani 1 1 d . . . H43A H 0.0511 0.4511 0.0070 0.191 Uiso 1 1 calc R . . H43B H -0.0340 0.4159 -0.0622 0.191 Uiso 1 1 calc R . . H43C H 0.1126 0.4146 -0.0199 0.191 Uiso 1 1 calc R . . C44 C 0.3479(8) 0.2797(3) 0.0893(6) 0.074(3) Uani 1 1 d . . . H44A H 0.3889 0.2981 0.0694 0.110 Uiso 1 1 calc R . . H44B H 0.3458 0.2484 0.0737 0.110 Uiso 1 1 calc R . . H44C H 0.3934 0.2819 0.1478 0.110 Uiso 1 1 calc R . . C45 C 0.1254(11) 0.3162(5) -0.0618(6) 0.136(6) Uani 1 1 d . . . H45A H 0.0358 0.3205 -0.0909 0.205 Uiso 1 1 calc R . . H45B H 0.1442 0.2922 -0.0873 0.205 Uiso 1 1 calc R . . H45C H 0.1646 0.3441 -0.0629 0.205 Uiso 1 1 calc R . . C46 C 0.0900(11) 0.2493(4) 0.0362(8) 0.140(6) Uani 1 1 d . . . H46A H 0.1021 0.2430 0.0885 0.210 Uiso 1 1 calc R . . H46B H 0.1164 0.2232 0.0190 0.210 Uiso 1 1 calc R . . H46C H 0.0025 0.2553 -0.0032 0.210 Uiso 1 1 calc R . . C47 C 0.6348(9) 0.3034(3) 0.6051(6) 0.085(4) Uani 1 1 d . . . H47A H 0.5841 0.3241 0.6136 0.127 Uiso 1 1 calc R . . H47B H 0.6471 0.2755 0.6348 0.127 Uiso 1 1 calc R . . H47C H 0.5931 0.2966 0.5478 0.127 Uiso 1 1 calc R . . C48 C 0.8348(11) 0.3580(3) 0.7404(6) 0.095(4) Uani 1 1 d . . . H48A H 0.9184 0.3702 0.7660 0.142 Uiso 1 1 calc R . . H48B H 0.8323 0.3358 0.7758 0.142 Uiso 1 1 calc R . . H48C H 0.7768 0.3824 0.7299 0.142 Uiso 1 1 calc R . . C49 C 0.9043(10) 0.2823(3) 0.6682(7) 0.102(4) Uani 1 1 d . . . H49A H 0.9828 0.2946 0.6797 0.152 Uiso 1 1 calc R . . H49B H 0.8711 0.2614 0.6229 0.152 Uiso 1 1 calc R . . H49C H 0.9179 0.2664 0.7155 0.152 Uiso 1 1 calc R . . C50 C 0.8711(9) 0.4348(3) 0.5044(6) 0.079(3) Uani 1 1 d . . . H50A H 0.8967 0.4137 0.4782 0.119 Uiso 1 1 calc R . . H50B H 0.9222 0.4619 0.5199 0.119 Uiso 1 1 calc R . . H50C H 0.7843 0.4429 0.4672 0.119 Uiso 1 1 calc R . . C51 C 1.0539(9) 0.3838(4) 0.6555(6) 0.096(4) Uani 1 1 d . . . H51A H 1.0736 0.3730 0.7078 0.144 Uiso 1 1 calc R . . H51B H 1.1126 0.4073 0.6634 0.144 Uiso 1 1 calc R . . H51C H 1.0595 0.3589 0.6255 0.144 Uiso 1 1 calc R . . C52 C 0.8876(11) 0.4554(3) 0.6606(6) 0.092(4) Uani 1 1 d . . . H52A H 0.8039 0.4678 0.6338 0.138 Uiso 1 1 calc R . . H52B H 0.9452 0.4790 0.6670 0.138 Uiso 1 1 calc R . . H52C H 0.9120 0.4438 0.7135 0.138 Uiso 1 1 calc R . . C53 C 0.5000 0.0000 0.5000 0.39(6) Uani 1 2 d S . . C54 C 0.386(7) -0.0179(15) 0.488(3) 0.37(3) Uani 1 1 d . . . C55 C 0.306(5) 0.0242(13) 0.429(2) 0.37(3) 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 Sm1 0.0283(2) 0.0339(3) 0.0316(3) -0.0037(2) 0.0145(2) -0.0011(2) Sm2 0.0293(2) 0.0359(3) 0.0327(3) -0.0026(2) 0.0145(2) 0.0026(2) Si1 0.0401(16) 0.085(2) 0.0443(19) -0.0069(16) 0.0140(15) -0.0013(15) Si2 0.0439(17) 0.098(2) 0.045(2) -0.0248(17) 0.0198(15) -0.0155(16) Si3 0.0520(17) 0.066(2) 0.0392(18) 0.0058(15) 0.0138(15) 0.0182(15) Si4 0.0408(16) 0.082(2) 0.0414(18) -0.0063(16) 0.0155(14) 0.0041(15) N5 0.041(4) 0.061(5) 0.032(4) -0.007(4) 0.020(4) -0.013(4) N6 0.036(4) 0.053(5) 0.030(4) 0.000(4) 0.010(3) 0.010(4) N1 0.035(4) 0.028(4) 0.032(4) -0.001(3) 0.019(4) 0.001(3) N2 0.036(4) 0.029(4) 0.038(5) -0.007(3) 0.022(4) 0.001(3) N3 0.036(4) 0.029(4) 0.031(4) -0.004(3) 0.017(4) -0.004(3) N4 0.030(4) 0.034(4) 0.036(5) 0.004(3) 0.022(4) 0.003(3) C10 0.040(5) 0.029(5) 0.039(6) 0.005(4) 0.021(5) -0.001(4) C9 0.049(6) 0.040(6) 0.043(6) -0.010(5) 0.023(5) -0.014(4) C8 0.033(5) 0.047(6) 0.050(6) 0.001(5) 0.024(5) 0.005(4) C7 0.040(5) 0.025(5) 0.040(6) 0.001(4) 0.021(5) -0.002(4) C1 0.030(5) 0.052(6) 0.033(5) 0.002(5) 0.017(4) 0.009(4) C2 0.029(5) 0.051(6) 0.047(6) -0.002(5) 0.025(5) -0.002(4) C3 0.037(5) 0.065(7) 0.059(7) -0.002(6) 0.025(5) 0.016(5) C4 0.080(8) 0.080(8) 0.057(8) -0.017(6) 0.052(7) -0.005(6) C5 0.052(6) 0.070(7) 0.051(7) 0.005(6) 0.034(5) 0.001(5) C6 0.044(5) 0.044(6) 0.032(5) -0.007(4) 0.022(5) -0.006(4) C40 0.026(4) 0.028(5) 0.031(5) 0.004(4) 0.016(4) 0.003(4) C39 0.047(5) 0.032(5) 0.042(6) 0.004(4) 0.025(5) 0.008(4) C38 0.028(5) 0.037(5) 0.043(6) -0.005(4) 0.020(5) -0.004(4) C37 0.026(4) 0.027(5) 0.034(5) 0.001(4) 0.014(4) -0.002(4) C31 0.034(5) 0.033(5) 0.040(6) 0.000(4) 0.022(5) 0.001(4) C32 0.044(5) 0.034(5) 0.047(6) -0.001(4) 0.026(5) -0.002(4) C33 0.061(7) 0.045(6) 0.051(7) 0.002(5) 0.025(6) 0.011(5) C34 0.066(7) 0.050(7) 0.069(8) 0.010(6) 0.034(6) -0.002(6) C35 0.061(7) 0.051(6) 0.055(7) -0.001(5) 0.033(6) -0.022(5) C36 0.035(5) 0.032(5) 0.054(6) -0.003(4) 0.024(5) -0.008(4) C30 0.027(5) 0.033(5) 0.045(6) 0.000(4) 0.019(5) -0.007(4) C29 0.028(5) 0.047(6) 0.037(6) 0.005(5) 0.016(4) -0.001(4) C28 0.041(5) 0.045(6) 0.036(6) -0.010(4) 0.025(5) -0.007(4) C27 0.031(5) 0.038(5) 0.030(5) -0.001(4) 0.016(4) -0.009(4) C21 0.022(4) 0.049(6) 0.039(5) -0.011(5) 0.015(4) -0.001(4) C26 0.035(5) 0.061(6) 0.041(6) -0.020(5) 0.018(5) -0.010(4) C25 0.039(6) 0.091(8) 0.065(8) -0.001(7) 0.026(6) -0.019(5) C24 0.068(8) 0.120(10) 0.061(8) 0.000(7) 0.045(7) -0.009(7) C23 0.054(6) 0.093(8) 0.041(6) -0.013(6) 0.032(5) -0.006(6) C22 0.034(5) 0.068(7) 0.051(7) -0.017(5) 0.023(5) 0.002(5) C20 0.033(5) 0.031(5) 0.040(6) -0.001(4) 0.021(5) 0.003(4) C19 0.022(5) 0.044(6) 0.050(6) 0.003(5) 0.003(5) 0.016(4) C18 0.047(6) 0.037(6) 0.045(6) 0.003(5) 0.016(5) 0.012(5) C17 0.042(5) 0.034(5) 0.050(6) -0.001(5) 0.030(5) 0.006(4) C11 0.054(6) 0.038(5) 0.023(6) 0.002(4) 0.018(5) 0.004(4) C12 0.062(6) 0.041(6) 0.044(6) -0.002(5) 0.033(5) 0.005(5) C13 0.097(8) 0.041(6) 0.049(7) -0.008(5) 0.042(7) 0.007(6) C14 0.092(8) 0.044(6) 0.064(8) 0.006(6) 0.044(7) -0.005(6) C15 0.087(8) 0.050(7) 0.055(7) 0.007(6) 0.044(7) 0.008(6) C16 0.065(7) 0.040(6) 0.048(7) 0.002(5) 0.030(6) 0.003(5) C41 0.041(7) 0.175(13) 0.119(12) -0.074(10) 0.023(7) -0.013(8) C42 0.070(7) 0.071(7) 0.072(8) -0.004(6) 0.042(7) 0.000(6) C43 0.145(13) 0.148(13) 0.079(10) 0.050(9) 0.055(10) 0.055(10) C44 0.058(7) 0.060(7) 0.082(9) -0.014(6) 0.025(6) -0.005(5) C45 0.123(12) 0.229(16) 0.052(9) 0.023(10) 0.044(9) 0.095(11) C46 0.111(11) 0.167(13) 0.174(15) -0.119(12) 0.098(12) -0.086(10) C47 0.079(8) 0.078(8) 0.076(9) 0.018(7) 0.027(7) 0.001(6) C48 0.119(10) 0.093(9) 0.055(8) 0.002(7) 0.037(8) 0.004(8) C49 0.094(9) 0.097(9) 0.109(11) 0.040(8) 0.052(9) 0.059(8) C50 0.082(8) 0.100(9) 0.051(8) 0.001(7) 0.033(7) -0.001(7) C51 0.049(7) 0.134(11) 0.082(10) 0.041(8) 0.021(7) 0.028(7) C52 0.110(10) 0.102(9) 0.068(9) -0.036(7) 0.051(8) -0.040(8) C53 0.56(14) 0.24(7) 0.66(14) -0.18(9) 0.53(14) -0.19(9) C54 0.58(9) 0.22(4) 0.29(5) -0.11(3) 0.23(6) -0.10(5) C55 0.71(9) 0.18(3) 0.45(6) 0.01(3) 0.47(7) 0.06(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N5 2.301(7) . ? Sm1 N2 2.655(6) . ? Sm1 N4 2.697(6) . ? Sm1 N1 2.726(6) . ? Sm1 N3 2.736(6) . ? Sm1 C10 2.834(8) . ? Sm1 C30 2.839(7) . ? Sm1 C7 2.850(8) . ? Sm1 C27 2.874(7) . ? Sm1 C29 2.880(8) . ? Sm1 C28 2.887(8) . ? Sm1 C9 2.916(8) . ? Sm2 N6 2.306(6) . ? Sm2 N1 2.668(6) . ? Sm2 N3 2.706(7) . ? Sm2 N2 2.725(6) . ? Sm2 N4 2.733(6) . ? Sm2 C20 2.817(8) . ? Sm2 C40 2.829(7) . ? Sm2 C17 2.848(8) . ? Sm2 C37 2.862(7) . ? Sm2 C39 2.891(8) . ? Sm2 C19 2.918(8) . ? Sm2 C38 2.921(7) . ? Si1 N5 1.708(7) . ? Si1 C42 1.858(9) . ? Si1 C43 1.860(11) . ? Si1 C41 1.866(10) . ? Si2 N5 1.713(7) . ? Si2 C45 1.837(11) . ? Si2 C44 1.840(9) . ? Si2 C46 1.874(11) . ? Si3 N6 1.715(7) . ? Si3 C47 1.851(10) . ? Si3 C48 1.867(10) . ? Si3 C49 1.871(9) . ? Si4 N6 1.703(7) . ? Si4 C50 1.861(10) . ? Si4 C51 1.864(9) . ? Si4 C52 1.880(10) . ? N1 C7 1.390(9) . ? N1 C10 1.391(9) . ? N2 C17 1.384(10) . ? N2 C20 1.387(9) . ? N3 C27 1.390(9) . ? N3 C30 1.390(9) . ? N4 C37 1.386(9) . ? N4 C40 1.392(9) . ? C10 C9 1.378(10) . ? C10 C11 1.514(11) . ? C9 C8 1.402(10) . ? C9 H9 0.9300 . ? C8 C7 1.380(10) . ? C8 H8 0.9300 . ? C7 C1 1.511(10) . ? C1 C40 1.505(10) . ? C1 C6 1.540(10) . ? C1 C2 1.548(10) . ? C2 C3 1.525(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.500(11) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.504(11) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.520(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C40 C39 1.367(10) . ? C39 C38 1.411(10) . ? C39 H39 0.9300 . ? C38 C37 1.374(10) . ? C38 H38 0.9300 . ? C37 C31 1.506(10) . ? C31 C30 1.513(11) . ? C31 C36 1.525(10) . ? C31 C32 1.560(10) . ? C32 C33 1.543(11) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.521(11) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.527(11) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.517(10) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C30 C29 1.367(10) . ? C29 C28 1.413(10) . ? C29 H29 0.9300 . ? C28 C27 1.382(10) . ? C28 H28 0.9300 . ? C27 C21 1.498(10) . ? C21 C20 1.503(11) . ? C21 C26 1.543(10) . ? C21 C22 1.546(10) . ? C26 C25 1.516(11) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C25 C24 1.505(12) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C24 C23 1.546(12) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C23 C22 1.506(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C20 C19 1.364(11) . ? C19 C18 1.416(11) . ? C19 H19 0.9300 . ? C18 C17 1.379(11) . ? C18 H18 0.9300 . ? C17 C11 1.513(11) . ? C11 C16 1.517(11) . ? C11 C12 1.552(10) . ? C12 C13 1.525(11) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.497(11) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.519(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.506(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.43(6) . ? C53 C54 1.43(6) 3_656 ? C54 C55 1.61(6) . ? 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 N5 Sm1 N2 126.6(2) . . ? N5 Sm1 N4 131.3(2) . . ? N2 Sm1 N4 102.08(19) . . ? N5 Sm1 N1 130.1(2) . . ? N2 Sm1 N1 66.41(19) . . ? N4 Sm1 N1 65.91(19) . . ? N5 Sm1 N3 130.0(2) . . ? N2 Sm1 N3 66.22(18) . . ? N4 Sm1 N3 65.91(18) . . ? N1 Sm1 N3 99.81(19) . . ? N5 Sm1 C10 108.9(2) . . ? N2 Sm1 C10 59.6(2) . . ? N4 Sm1 C10 94.7(2) . . ? N1 Sm1 C10 28.89(19) . . ? N3 Sm1 C10 116.2(2) . . ? N5 Sm1 C30 111.0(2) . . ? N2 Sm1 C30 94.9(2) . . ? N4 Sm1 C30 58.7(2) . . ? N1 Sm1 C30 115.5(2) . . ? N3 Sm1 C30 28.81(18) . . ? C10 Sm1 C30 140.1(2) . . ? N5 Sm1 C7 111.5(2) . . ? N2 Sm1 C7 95.1(2) . . ? N4 Sm1 C7 58.1(2) . . ? N1 Sm1 C7 28.77(18) . . ? N3 Sm1 C7 115.0(2) . . ? C10 Sm1 C7 45.6(2) . . ? C30 Sm1 C7 116.8(2) . . ? N5 Sm1 C27 109.8(2) . . ? N2 Sm1 C27 58.3(2) . . ? N4 Sm1 C27 94.4(2) . . ? N1 Sm1 C27 115.1(2) . . ? N3 Sm1 C27 28.55(19) . . ? C10 Sm1 C27 117.8(2) . . ? C30 Sm1 C27 45.7(2) . . ? C7 Sm1 C27 138.7(2) . . ? N5 Sm1 C29 85.0(2) . . ? N2 Sm1 C29 104.3(2) . . ? N4 Sm1 C29 82.8(2) . . ? N1 Sm1 C29 143.2(2) . . ? N3 Sm1 C29 47.4(2) . . ? C10 Sm1 C29 162.9(2) . . ? C30 Sm1 C29 27.6(2) . . ? C7 Sm1 C29 139.3(2) . . ? C27 Sm1 C29 46.0(2) . . ? N5 Sm1 C28 84.2(2) . . ? N2 Sm1 C28 82.0(2) . . ? N4 Sm1 C28 104.6(2) . . ? N1 Sm1 C28 142.9(2) . . ? N3 Sm1 C28 47.3(2) . . ? C10 Sm1 C28 140.0(2) . . ? C30 Sm1 C28 45.9(2) . . ? C7 Sm1 C28 161.6(2) . . ? C27 Sm1 C28 27.8(2) . . ? C29 Sm1 C28 28.4(2) . . ? N5 Sm1 C9 84.0(2) . . ? N2 Sm1 C9 84.0(2) . . ? N4 Sm1 C9 103.2(2) . . ? N1 Sm1 C9 47.2(2) . . ? N3 Sm1 C9 143.8(2) . . ? C10 Sm1 C9 27.7(2) . . ? C30 Sm1 C9 161.4(3) . . ? C7 Sm1 C9 45.1(2) . . ? C27 Sm1 C9 141.1(2) . . ? C29 Sm1 C9 168.8(2) . . ? C28 Sm1 C9 150.9(2) . . ? N6 Sm2 N1 126.9(2) . . ? N6 Sm2 N3 131.0(2) . . ? N1 Sm2 N3 102.06(19) . . ? N6 Sm2 N2 130.3(2) . . ? N1 Sm2 N2 66.25(19) . . ? N3 Sm2 N2 65.68(19) . . ? N6 Sm2 N4 130.3(2) . . ? N1 Sm2 N4 66.20(18) . . ? N3 Sm2 N4 65.83(19) . . ? N2 Sm2 N4 99.37(19) . . ? N6 Sm2 C20 110.8(2) . . ? N1 Sm2 C20 95.0(2) . . ? N3 Sm2 C20 58.8(2) . . ? N2 Sm2 C20 28.92(18) . . ? N4 Sm2 C20 115.5(2) . . ? N6 Sm2 C40 109.2(2) . . ? N1 Sm2 C40 59.2(2) . . ? N3 Sm2 C40 94.6(2) . . ? N2 Sm2 C40 115.8(2) . . ? N4 Sm2 C40 28.93(18) . . ? C20 Sm2 C40 140.0(2) . . ? N6 Sm2 C17 110.0(2) . . ? N1 Sm2 C17 58.6(2) . . ? N3 Sm2 C17 94.3(2) . . ? N2 Sm2 C17 28.7(2) . . ? N4 Sm2 C17 115.0(2) . . ? C20 Sm2 C17 45.5(2) . . ? C40 Sm2 C17 117.7(2) . . ? N6 Sm2 C37 111.5(2) . . ? N1 Sm2 C37 94.7(2) . . ? N3 Sm2 C37 58.2(2) . . ? N2 Sm2 C37 114.6(2) . . ? N4 Sm2 C37 28.56(17) . . ? C20 Sm2 C37 116.9(2) . . ? C40 Sm2 C37 45.4(2) . . ? C17 Sm2 C37 138.5(2) . . ? N6 Sm2 C39 84.2(2) . . ? N1 Sm2 C39 83.5(2) . . ? N3 Sm2 C39 103.3(2) . . ? N2 Sm2 C39 143.3(2) . . ? N4 Sm2 C39 47.2(2) . . ? C20 Sm2 C39 161.5(2) . . ? C40 Sm2 C39 27.6(2) . . ? C17 Sm2 C39 140.9(2) . . ? C37 Sm2 C39 45.1(2) . . ? N6 Sm2 C19 85.2(2) . . ? N1 Sm2 C19 103.9(2) . . ? N3 Sm2 C19 82.8(2) . . ? N2 Sm2 C19 47.2(2) . . ? N4 Sm2 C19 142.8(2) . . ? C20 Sm2 C19 27.4(2) . . ? C40 Sm2 C19 162.1(2) . . ? C17 Sm2 C19 45.4(2) . . ? C37 Sm2 C19 139.7(2) . . ? C39 Sm2 C19 169.4(2) . . ? N6 Sm2 C38 85.4(2) . . ? N1 Sm2 C38 105.2(2) . . ? N3 Sm2 C38 81.5(2) . . ? N2 Sm2 C38 142.1(2) . . ? N4 Sm2 C38 47.5(2) . . ? C20 Sm2 C38 138.5(2) . . ? C40 Sm2 C38 46.2(2) . . ? C17 Sm2 C38 162.2(2) . . ? C37 Sm2 C38 27.5(2) . . ? C39 Sm2 C38 28.10(19) . . ? C19 Sm2 C38 149.2(2) . . ? N5 Si1 C42 109.0(4) . . ? N5 Si1 C43 113.0(5) . . ? C42 Si1 C43 106.7(5) . . ? N5 Si1 C41 114.2(4) . . ? C42 Si1 C41 107.8(5) . . ? C43 Si1 C41 105.8(6) . . ? N5 Si2 C45 115.3(5) . . ? N5 Si2 C44 109.8(4) . . ? C45 Si2 C44 106.7(5) . . ? N5 Si2 C46 114.0(4) . . ? C45 Si2 C46 104.2(6) . . ? C44 Si2 C46 106.2(5) . . ? N6 Si3 C47 110.2(4) . . ? N6 Si3 C48 114.4(4) . . ? C47 Si3 C48 104.4(5) . . ? N6 Si3 C49 113.8(4) . . ? C47 Si3 C49 106.9(5) . . ? C48 Si3 C49 106.5(5) . . ? N6 Si4 C50 109.9(4) . . ? N6 Si4 C51 113.3(4) . . ? C50 Si4 C51 105.8(5) . . ? N6 Si4 C52 114.3(4) . . ? C50 Si4 C52 106.2(5) . . ? C51 Si4 C52 106.7(5) . . ? Si1 N5 Si2 120.7(4) . . ? Si1 N5 Sm1 119.0(3) . . ? Si2 N5 Sm1 120.3(4) . . ? Si4 N6 Si3 119.3(4) . . ? Si4 N6 Sm2 120.0(4) . . ? Si3 N6 Sm2 120.6(4) . . ? C7 N1 C10 104.7(7) . . ? C7 N1 Sm2 122.3(5) . . ? C10 N1 Sm2 123.8(5) . . ? C7 N1 Sm1 80.6(4) . . ? C10 N1 Sm1 79.9(4) . . ? Sm2 N1 Sm1 79.48(16) . . ? C17 N2 C20 104.4(7) . . ? C17 N2 Sm1 122.4(5) . . ? C20 N2 Sm1 123.8(5) . . ? C17 N2 Sm2 80.6(5) . . ? C20 N2 Sm2 79.2(4) . . ? Sm1 N2 Sm2 79.70(16) . . ? C27 N3 C30 105.8(7) . . ? C27 N3 Sm2 121.9(5) . . ? C30 N3 Sm2 122.9(5) . . ? C27 N3 Sm1 81.3(4) . . ? C30 N3 Sm1 79.7(4) . . ? Sm2 N3 Sm1 78.65(16) . . ? C37 N4 C40 104.6(7) . . ? C37 N4 Sm1 122.6(5) . . ? C40 N4 Sm1 123.1(5) . . ? C37 N4 Sm2 80.9(4) . . ? C40 N4 Sm2 79.3(4) . . ? Sm1 N4 Sm2 78.84(16) . . ? C9 C10 N1 109.7(7) . . ? C9 C10 C11 135.6(8) . . ? N1 C10 C11 114.4(7) . . ? C9 C10 Sm1 79.5(5) . . ? N1 C10 Sm1 71.3(4) . . ? C11 C10 Sm1 119.3(5) . . ? C10 C9 C8 108.3(8) . . ? C10 C9 Sm1 72.8(5) . . ? C8 C9 Sm1 77.1(5) . . ? C10 C9 H9 125.9 . . ? C8 C9 H9 125.9 . . ? Sm1 C9 H9 116.2 . . ? C7 C8 C9 105.5(7) . . ? C7 C8 Sm1 72.6(5) . . ? C9 C8 Sm1 75.2(5) . . ? C7 C8 H8 127.3 . . ? C9 C8 H8 127.3 . . ? Sm1 C8 H8 117.3 . . ? C8 C7 N1 111.4(7) . . ? C8 C7 C1 133.3(8) . . ? N1 C7 C1 114.9(7) . . ? C8 C7 Sm1 79.9(5) . . ? N1 C7 Sm1 70.7(4) . . ? C1 C7 Sm1 120.9(5) . . ? C40 C1 C7 104.4(6) . . ? C40 C1 C6 116.8(7) . . ? C7 C1 C6 106.4(7) . . ? C40 C1 C2 109.0(6) . . ? C7 C1 C2 113.0(7) . . ? C6 C1 C2 107.3(6) . . ? C3 C2 C1 111.6(7) . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? C3 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 112.7(8) . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 C5 110.5(7) . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 112.1(8) . . ? C4 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C5 C6 C1 115.1(7) . . ? C5 C6 H6A 108.5 . . ? C1 C6 H6A 108.5 . . ? C5 C6 H6B 108.5 . . ? C1 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? C39 C40 N4 109.6(7) . . ? C39 C40 C1 135.8(8) . . ? N4 C40 C1 114.2(7) . . ? C39 C40 Sm2 78.7(5) . . ? N4 C40 Sm2 71.7(4) . . ? C1 C40 Sm2 119.8(5) . . ? C40 C39 C38 108.5(8) . . ? C40 C39 Sm2 73.7(5) . . ? C38 C39 Sm2 77.1(4) . . ? C40 C39 H39 125.7 . . ? C38 C39 H39 125.7 . . ? Sm2 C39 H39 115.6 . . ? C37 C38 C39 104.9(7) . . ? C37 C38 Sm2 73.9(5) . . ? C39 C38 Sm2 74.8(4) . . ? C37 C38 H38 127.6 . . ? C39 C38 H38 127.6 . . ? Sm2 C38 H38 116.3 . . ? C38 C37 N4 111.8(7) . . ? C38 C37 C31 133.4(7) . . ? N4 C37 C31 114.7(7) . . ? C38 C37 Sm2 78.6(5) . . ? N4 C37 Sm2 70.5(4) . . ? C31 C37 Sm2 120.3(5) . . ? C37 C31 C30 105.0(6) . . ? C37 C31 C36 113.9(7) . . ? C30 C31 C36 110.0(6) . . ? C37 C31 C32 106.5(6) . . ? C30 C31 C32 114.4(7) . . ? C36 C31 C32 107.2(6) . . ? C33 C32 C31 114.7(7) . . ? C33 C32 H32A 108.6 . . ? C31 C32 H32A 108.6 . . ? C33 C32 H32B 108.6 . . ? C31 C32 H32B 108.6 . . ? H32A C32 H32B 107.6 . . ? C34 C33 C32 110.2(8) . . ? C34 C33 H33A 109.6 . . ? C32 C33 H33A 109.6 . . ? C34 C33 H33B 109.6 . . ? C32 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? C33 C34 C35 110.8(7) . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C36 C35 C34 110.4(7) . . ? C36 C35 H35A 109.6 . . ? C34 C35 H35A 109.6 . . ? C36 C35 H35B 109.6 . . ? C34 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? C35 C36 C31 113.9(7) . . ? C35 C36 H36A 108.8 . . ? C31 C36 H36A 108.8 . . ? C35 C36 H36B 108.8 . . ? C31 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C29 C30 N3 110.1(7) . . ? C29 C30 C31 135.8(8) . . ? N3 C30 C31 113.9(7) . . ? C29 C30 Sm1 77.9(5) . . ? N3 C30 Sm1 71.5(4) . . ? C31 C30 Sm1 120.1(5) . . ? C30 C29 C28 107.0(8) . . ? C30 C29 Sm1 74.5(5) . . ? C28 C29 Sm1 76.1(4) . . ? C30 C29 H29 126.5 . . ? C28 C29 H29 126.5 . . ? Sm1 C29 H29 115.3 . . ? C27 C28 C29 107.0(8) . . ? C27 C28 Sm1 75.6(5) . . ? C29 C28 Sm1 75.6(5) . . ? C27 C28 H28 126.5 . . ? C29 C28 H28 126.5 . . ? Sm1 C28 H28 114.7 . . ? C28 C27 N3 109.3(7) . . ? C28 C27 C21 136.2(8) . . ? N3 C27 C21 114.5(7) . . ? C28 C27 Sm1 76.6(5) . . ? N3 C27 Sm1 70.2(4) . . ? C21 C27 Sm1 119.7(5) . . ? C27 C21 C20 104.9(6) . . ? C27 C21 C26 109.0(7) . . ? C20 C21 C26 112.1(7) . . ? C27 C21 C22 116.0(7) . . ? C20 C21 C22 108.0(7) . . ? C26 C21 C22 107.0(6) . . ? C25 C26 C21 112.3(7) . . ? C25 C26 H26A 109.1 . . ? C21 C26 H26A 109.1 . . ? C25 C26 H26B 109.1 . . ? C21 C26 H26B 109.1 . . ? H26A C26 H26B 107.9 . . ? C24 C25 C26 111.7(8) . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? C25 C24 C23 110.3(8) . . ? C25 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? C25 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C22 C23 C24 111.5(8) . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? C23 C22 C21 115.4(7) . . ? C23 C22 H22A 108.4 . . ? C21 C22 H22A 108.4 . . ? C23 C22 H22B 108.4 . . ? C21 C22 H22B 108.4 . . ? H22A C22 H22B 107.5 . . ? C19 C20 N2 110.9(8) . . ? C19 C20 C21 133.7(8) . . ? N2 C20 C21 114.8(7) . . ? C19 C20 Sm2 80.4(5) . . ? N2 C20 Sm2 71.9(4) . . ? C21 C20 Sm2 120.2(5) . . ? C20 C19 C18 107.4(8) . . ? C20 C19 Sm2 72.2(5) . . ? C18 C19 Sm2 77.2(5) . . ? C20 C19 H19 126.3 . . ? C18 C19 H19 126.3 . . ? Sm2 C19 H19 116.4 . . ? C17 C18 C19 105.5(8) . . ? C17 C18 Sm2 72.2(5) . . ? C19 C18 Sm2 74.9(4) . . ? C17 C18 H18 127.3 . . ? C19 C18 H18 127.3 . . ? Sm2 C18 H18 117.9 . . ? C18 C17 N2 111.5(8) . . ? C18 C17 C11 132.0(8) . . ? N2 C17 C11 116.2(7) . . ? C18 C17 Sm2 80.3(5) . . ? N2 C17 Sm2 70.8(4) . . ? C11 C17 Sm2 120.0(5) . . ? C17 C11 C10 104.1(6) . . ? C17 C11 C16 112.6(7) . . ? C10 C11 C16 109.9(7) . . ? C17 C11 C12 108.7(7) . . ? C10 C11 C12 113.6(7) . . ? C16 C11 C12 107.9(7) . . ? C13 C12 C11 115.3(7) . . ? C13 C12 H12A 108.5 . . ? C11 C12 H12A 108.5 . . ? C13 C12 H12B 108.5 . . ? C11 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C14 C13 C12 110.0(8) . . ? C14 C13 H13A 109.7 . . ? C12 C13 H13A 109.7 . . ? C14 C13 H13B 109.7 . . ? C12 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C13 C14 C15 112.0(8) . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14B 109.2 . . ? C15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 110.1(8) . . ? C16 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? C16 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C15 C16 C11 113.6(8) . . ? C15 C16 H16A 108.8 . . ? C11 C16 H16A 108.8 . . ? C15 C16 H16B 108.8 . . ? C11 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? Si1 C41 H41A 109.5 . . ? Si1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si1 C42 H42A 109.5 . . ? Si1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si2 C44 H44A 109.5 . . ? Si2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si2 C45 H45A 109.5 . . ? Si2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si2 C46 H46A 109.5 . . ? Si2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? Si3 C47 H47A 109.5 . . ? Si3 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si3 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Si3 C48 H48A 109.5 . . ? Si3 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si3 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Si3 C49 H49A 109.5 . . ? Si3 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? Si3 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? Si4 C50 H50A 109.5 . . ? Si4 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Si4 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Si4 C51 H51A 109.5 . . ? Si4 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si4 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si4 C52 H52A 109.5 . . ? Si4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C54 180(4) . 3_656 ? C53 C54 C55 91(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.780 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.141