# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Shuangliu, Zhou' _publ_contact_author_email swwang@mail.ahnu.edu.cn _publ_section_title ; Rare Earth Metal Bis(trimethylsilyl)amido Complexes Bearing Pyrrolyl-methylamide Ligand. Synthesis, Structure, and Catalytic Activity towards Guanylation of Amines ; loop_ _publ_author_name 'Liu Chao' 'Zhou Shuangliu' 'Wang Shaowu' 'Zhang Lijun' 'Yang Gaosheng' # Attachment '- Supporting Information.txt' data_ccdc-770560 _database_code_depnum_ccdc_archive 'CCDC 770560' #TrackingRef '- Supporting Information.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H68 N6 Si4 Y2' _chemical_formula_weight 923.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.4503(9) _cell_length_b 14.9010(11) _cell_length_c 26.724(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4957.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6684 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 22.43 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 2.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.759939 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS-2004/1 - Bruker Nonius area detector scaling and absorption correction' _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 36612 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4873 _reflns_number_gt 2733 _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. The restraints of DFIX, DELU, SIMU and ISOR were used. ; _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^)+(0.0617P)^2^+0.4390P] 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 4873 _refine_ls_number_parameters 269 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.045 _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 Y1 Y 0.46069(3) -0.06140(3) 0.564182(14) 0.05263(15) Uani 1 1 d . . . N1 N 0.4389(2) 0.1735(2) 0.46031(12) 0.0555(8) Uani 1 1 d . . . N2 N 0.3852(2) -0.0034(2) 0.47517(12) 0.0569(8) Uani 1 1 d . . . N3 N 0.4193(3) -0.0658(2) 0.64432(12) 0.0737(10) Uani 1 1 d . A . Si1 Si 0.34419(15) -0.15179(11) 0.66779(6) 0.1072(6) Uani 1 1 d D . . Si2 Si 0.45838(12) 0.02805(11) 0.67632(5) 0.0855(4) Uani 1 1 d . . . C1 C 0.4057(6) 0.5214(3) 0.3688(2) 0.125(2) Uani 1 1 d . . . H1A H 0.3624 0.5175 0.3392 0.188 Uiso 1 1 calc R . . H1B H 0.4769 0.5402 0.3600 0.188 Uiso 1 1 calc R . . H1C H 0.3746 0.5642 0.3914 0.188 Uiso 1 1 calc R . . C2 C 0.4106(4) 0.4301(3) 0.3940(2) 0.0804(14) Uani 1 1 d . . . C3 C 0.4690(3) 0.4182(3) 0.43755(18) 0.0717(13) Uani 1 1 d . . . H3A H 0.5038 0.4674 0.4516 0.086 Uiso 1 1 calc R . . C4 C 0.4772(3) 0.3355(3) 0.46085(16) 0.0593(10) Uani 1 1 d . . . C5 C 0.5428(3) 0.3265(3) 0.50798(18) 0.0809(14) Uani 1 1 d . . . H5A H 0.5718 0.3840 0.5169 0.121 Uiso 1 1 calc R . . H5B H 0.6005 0.2849 0.5024 0.121 Uiso 1 1 calc R . . H5C H 0.4979 0.3050 0.5346 0.121 Uiso 1 1 calc R . . C6 C 0.4263(3) 0.2610(3) 0.43987(15) 0.0569(10) Uani 1 1 d . . . C7 C 0.3657(3) 0.2733(3) 0.39665(17) 0.0710(12) Uani 1 1 d . . . C8 C 0.3585(4) 0.3568(4) 0.37506(18) 0.0812(13) Uani 1 1 d . . . H8A H 0.3167 0.3636 0.3465 0.097 Uiso 1 1 calc R . . C9 C 0.3072(5) 0.1942(3) 0.3729(2) 0.112(2) Uani 1 1 d . . . H9A H 0.3199 0.1411 0.3923 0.168 Uiso 1 1 calc R . . H9B H 0.3333 0.1853 0.3395 0.168 Uiso 1 1 calc R . . H9C H 0.2315 0.2064 0.3719 0.168 Uiso 1 1 calc R . . C10 C 0.3647(3) 0.1565(3) 0.50103(17) 0.0749(13) Uani 1 1 d . . . H10A H 0.2983 0.1886 0.4947 0.090 Uiso 1 1 calc R . . H10B H 0.3951 0.1796 0.5319 0.090 Uiso 1 1 calc R . . C11 C 0.3402(3) 0.0585(3) 0.50757(16) 0.0610(11) Uani 1 1 d . . . C12 C 0.2662(3) 0.0176(4) 0.53865(18) 0.0748(13) Uani 1 1 d . . . H12A H 0.2168 0.0481 0.5616 0.090 Uiso 1 1 calc R . . C13 C 0.2611(3) -0.0726(4) 0.52399(19) 0.0809(14) Uani 1 1 d . . . H13A H 0.2053 -0.1156 0.5337 0.097 Uiso 1 1 calc R . . C14 C 0.3344(4) -0.0839(3) 0.48566(17) 0.0696(12) Uani 1 1 d . . . H14A H 0.3366 -0.1366 0.4637 0.084 Uiso 1 1 calc R . . C15 C 0.4385(17) -0.2137(14) 0.7176(7) 0.135(7) Uani 0.402(16) 1 d PDU A 1 H15A H 0.5025 -0.2344 0.7012 0.202 Uiso 0.402(16) 1 calc PR A 1 H15B H 0.4008 -0.2640 0.7316 0.202 Uiso 0.402(16) 1 calc PR A 1 H15C H 0.4574 -0.1725 0.7437 0.202 Uiso 0.402(16) 1 calc PR A 1 C16 C 0.2295(15) -0.1291(13) 0.7028(9) 0.140(8) Uani 0.402(16) 1 d PDU A 1 H16A H 0.2481 -0.0915 0.7307 0.210 Uiso 0.402(16) 1 calc PR A 1 H16B H 0.1995 -0.1843 0.7149 0.210 Uiso 0.402(16) 1 calc PR A 1 H16C H 0.1778 -0.0988 0.6822 0.210 Uiso 0.402(16) 1 calc PR A 1 C17 C 0.323(2) -0.2337(16) 0.6178(8) 0.084(7) Uani 0.402(16) 1 d PDU A 1 H17A H 0.3417 -0.2072 0.5862 0.126 Uiso 0.402(16) 1 calc PR A 1 H17B H 0.2490 -0.2515 0.6173 0.126 Uiso 0.402(16) 1 calc PR A 1 H17C H 0.3674 -0.2853 0.6237 0.126 Uiso 0.402(16) 1 calc PR A 1 C15' C 0.3671(15) -0.1857(10) 0.7305(4) 0.147(6) Uani 0.598(16) 1 d PDU A 2 H15D H 0.4387 -0.2090 0.7335 0.221 Uiso 0.598(16) 1 calc PR A 2 H15E H 0.3164 -0.2315 0.7395 0.221 Uiso 0.598(16) 1 calc PR A 2 H15F H 0.3587 -0.1351 0.7523 0.221 Uiso 0.598(16) 1 calc PR A 2 C16' C 0.1922(8) -0.1119(9) 0.6670(6) 0.121(5) Uani 0.598(16) 1 d PDU A 2 H16D H 0.1875 -0.0520 0.6801 0.182 Uiso 0.598(16) 1 calc PR A 2 H16E H 0.1499 -0.1515 0.6874 0.182 Uiso 0.598(16) 1 calc PR A 2 H16F H 0.1657 -0.1128 0.6333 0.182 Uiso 0.598(16) 1 calc PR A 2 C17' C 0.3411(16) -0.2505(11) 0.6260(6) 0.094(5) Uani 0.598(16) 1 d PDU A 2 H17D H 0.3115 -0.2336 0.5942 0.141 Uiso 0.598(16) 1 calc PR A 2 H17E H 0.2974 -0.2966 0.6407 0.141 Uiso 0.598(16) 1 calc PR A 2 H17F H 0.4128 -0.2727 0.6214 0.141 Uiso 0.598(16) 1 calc PR A 2 C18 C 0.5683(6) 0.0077(5) 0.7208(3) 0.158(3) Uani 1 1 d . A . H18A H 0.5542 0.0394 0.7514 0.237 Uiso 1 1 calc R . . H18B H 0.6347 0.0285 0.7067 0.237 Uiso 1 1 calc R . . H18C H 0.5734 -0.0554 0.7276 0.237 Uiso 1 1 calc R . . C19 C 0.3484(6) 0.0848(4) 0.7107(2) 0.139(3) Uani 1 1 d . A . H19A H 0.3741 0.1039 0.7429 0.208 Uiso 1 1 calc R . . H19B H 0.2897 0.0438 0.7151 0.208 Uiso 1 1 calc R . . H19C H 0.3246 0.1361 0.6920 0.208 Uiso 1 1 calc R . . C20 C 0.5109(6) 0.1099(4) 0.6303(2) 0.132(2) Uani 1 1 d . A . H20A H 0.5285 0.1649 0.6470 0.199 Uiso 1 1 calc R . . H20B H 0.4573 0.1212 0.6052 0.199 Uiso 1 1 calc R . . H20C H 0.5742 0.0859 0.6147 0.199 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 Y1 0.0481(2) 0.0590(3) 0.0509(2) 0.0018(2) -0.00048(17) -0.00017(18) N1 0.0507(18) 0.059(2) 0.057(2) 0.0032(17) 0.0055(15) -0.0004(16) N2 0.0490(18) 0.063(2) 0.059(2) 0.0044(18) -0.0093(16) -0.0054(17) N3 0.077(2) 0.091(3) 0.053(2) -0.001(2) 0.0030(18) 0.007(2) Si1 0.1391(14) 0.1099(12) 0.0725(10) -0.0025(9) 0.0426(10) -0.0134(11) Si2 0.0980(11) 0.0989(10) 0.0595(8) -0.0059(8) -0.0080(7) 0.0126(9) C1 0.174(6) 0.072(3) 0.130(5) 0.024(4) 0.021(5) 0.029(4) C2 0.088(3) 0.076(4) 0.077(3) 0.014(3) 0.017(3) 0.022(3) C3 0.071(3) 0.053(3) 0.091(4) -0.005(3) 0.016(3) 0.001(2) C4 0.049(2) 0.062(3) 0.067(3) -0.004(2) 0.010(2) 0.004(2) C5 0.080(3) 0.073(3) 0.090(4) -0.011(3) -0.010(3) -0.006(3) C6 0.047(2) 0.060(3) 0.064(3) 0.001(2) 0.004(2) 0.0056(19) C7 0.070(3) 0.070(3) 0.073(3) 0.008(3) -0.010(2) 0.003(2) C8 0.086(3) 0.084(4) 0.073(3) 0.007(3) -0.011(3) 0.015(3) C9 0.125(5) 0.102(4) 0.109(4) 0.008(4) -0.059(4) -0.019(4) C10 0.068(3) 0.071(3) 0.086(3) 0.009(3) 0.015(2) 0.014(2) C11 0.045(2) 0.069(3) 0.069(3) 0.011(2) -0.004(2) 0.002(2) C12 0.045(2) 0.093(4) 0.087(3) 0.023(3) 0.005(2) 0.000(2) C13 0.049(2) 0.102(4) 0.092(4) 0.029(3) -0.012(3) -0.021(3) C14 0.061(3) 0.070(3) 0.077(3) 0.008(2) -0.024(2) -0.017(2) C15 0.154(11) 0.137(10) 0.113(10) 0.032(8) -0.004(8) 0.005(8) C16 0.143(11) 0.146(11) 0.131(11) -0.010(8) 0.044(8) 0.007(8) C17 0.088(10) 0.087(10) 0.077(9) 0.018(7) 0.005(7) -0.004(8) C15' 0.179(10) 0.157(9) 0.106(7) 0.022(6) 0.014(7) -0.022(8) C16' 0.098(6) 0.156(8) 0.110(8) -0.010(7) 0.041(6) 0.001(6) C17' 0.094(8) 0.093(8) 0.095(8) -0.006(7) 0.023(6) 0.005(6) C18 0.179(7) 0.155(6) 0.141(6) -0.028(5) -0.091(5) 0.021(5) C19 0.173(7) 0.109(5) 0.134(6) -0.025(4) 0.041(5) 0.020(5) C20 0.181(6) 0.118(5) 0.098(4) -0.013(4) -0.003(4) -0.059(5) _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 Y1 N1 2.186(3) 5_656 ? Y1 N3 2.204(3) . ? Y1 N2 2.392(3) 5_656 ? Y1 C14 2.644(4) . ? Y1 N2 2.700(3) . ? Y1 C13 2.712(4) . ? Y1 C12 2.777(4) . ? Y1 C11 2.781(4) . ? N1 C6 1.422(5) . ? N1 C10 1.450(5) . ? N1 Y1 2.186(3) 5_656 ? N2 C11 1.383(5) . ? N2 C14 1.385(5) . ? N2 Y1 2.392(3) 5_656 ? N3 Si1 1.706(4) . ? N3 Si2 1.710(4) . ? Si1 C16 1.741(12) . ? Si1 C15' 1.772(10) . ? Si1 C17 1.828(14) . ? Si1 C17' 1.848(11) . ? Si1 C16' 1.983(10) . ? Si1 C15 1.999(13) . ? Si2 C18 1.838(6) . ? Si2 C20 1.851(6) . ? Si2 C19 1.853(6) . ? C1 C2 1.519(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C8 1.368(6) . ? C2 C3 1.384(6) . ? C3 C4 1.385(6) . ? C3 H3A 0.9300 . ? C4 C6 1.396(6) . ? C4 C5 1.507(6) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.391(5) . ? C7 C8 1.374(6) . ? C7 C9 1.524(6) . ? C8 H8A 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.502(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.382(5) . ? C12 C13 1.402(6) . ? C12 H12A 0.9800 . ? C13 C14 1.382(6) . ? C13 H13A 0.9800 . ? C14 H14A 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C15' H15D 0.9600 . ? C15' H15E 0.9600 . ? C15' H15F 0.9600 . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17' H17D 0.9600 . ? C17' H17E 0.9600 . ? C17' H17F 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 . ? 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 N1 Y1 N3 113.69(13) 5_656 . ? N1 Y1 N2 73.62(11) 5_656 5_656 ? N3 Y1 N2 128.82(12) . 5_656 ? N1 Y1 C14 90.32(14) 5_656 . ? N3 Y1 C14 128.94(14) . . ? N2 Y1 C14 100.34(13) 5_656 . ? N1 Y1 N2 100.37(11) 5_656 . ? N3 Y1 N2 141.65(12) . . ? N2 Y1 N2 76.28(10) 5_656 . ? C14 Y1 N2 30.02(11) . . ? N1 Y1 C13 110.98(15) 5_656 . ? N3 Y1 C13 99.72(15) . . ? N2 Y1 C13 125.86(12) 5_656 . ? C14 Y1 C13 29.87(13) . . ? N2 Y1 C13 49.59(12) . . ? N1 Y1 C12 138.47(15) 5_656 . ? N3 Y1 C12 92.73(14) . . ? N2 Y1 C12 114.86(12) 5_656 . ? C14 Y1 C12 48.72(16) . . ? N2 Y1 C12 49.01(12) . . ? C13 Y1 C12 29.56(13) . . ? N1 Y1 C11 129.53(13) 5_656 . ? N3 Y1 C11 114.94(13) . . ? N2 Y1 C11 86.24(11) 5_656 . ? C14 Y1 C11 47.84(13) . . ? N2 Y1 C11 29.19(10) . . ? C13 Y1 C11 47.92(13) . . ? C12 Y1 C11 28.78(11) . . ? N1 Y1 Y1 87.31(9) 5_656 5_656 ? N3 Y1 Y1 154.44(9) . 5_656 ? N2 Y1 Y1 40.86(7) 5_656 5_656 ? C14 Y1 Y1 61.58(10) . 5_656 ? N2 Y1 Y1 35.42(6) . 5_656 ? C13 Y1 Y1 85.01(10) . 5_656 ? C12 Y1 Y1 78.99(9) . 5_656 ? C11 Y1 Y1 51.17(9) . 5_656 ? C6 N1 C10 112.2(3) . . ? C6 N1 Y1 130.4(2) . 5_656 ? C10 N1 Y1 117.1(2) . 5_656 ? C11 N2 C14 105.4(3) . . ? C11 N2 Y1 109.3(2) . 5_656 ? C14 N2 Y1 143.6(3) . 5_656 ? C11 N2 Y1 78.7(2) . . ? C14 N2 Y1 72.7(2) . . ? Y1 N2 Y1 103.72(10) 5_656 . ? Si1 N3 Si2 125.9(2) . . ? Si1 N3 Y1 120.52(19) . . ? Si2 N3 Y1 113.29(19) . . ? N3 Si1 C16 120.1(7) . . ? N3 Si1 C15' 118.3(5) . . ? C16 Si1 C15' 71.3(8) . . ? N3 Si1 C17 108.2(10) . . ? C16 Si1 C17 113.9(11) . . ? C15' Si1 C17 121.5(10) . . ? N3 Si1 C17' 112.8(7) . . ? C16 Si1 C17' 117.6(10) . . ? C15' Si1 C17' 110.3(7) . . ? C17 Si1 C17' 12.5(12) . . ? N3 Si1 C16' 107.1(4) . . ? C16 Si1 C16' 33.4(7) . . ? C15' Si1 C16' 104.4(5) . . ? C17 Si1 C16' 93.2(10) . . ? C17' Si1 C16' 102.3(7) . . ? N3 Si1 C15 105.6(7) . . ? C16 Si1 C15 102.3(8) . . ? C15' Si1 C15 31.3(5) . . ? C17 Si1 C15 105.2(9) . . ? C17' Si1 C15 92.7(9) . . ? C16' Si1 C15 134.8(6) . . ? N3 Si2 C18 113.6(3) . . ? N3 Si2 C20 107.8(2) . . ? C18 Si2 C20 106.0(4) . . ? N3 Si2 C19 114.3(3) . . ? C18 Si2 C19 107.7(3) . . ? C20 Si2 C19 106.9(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C8 C2 C3 117.3(4) . . ? C8 C2 C1 122.2(5) . . ? C3 C2 C1 120.5(5) . . ? C2 C3 C4 122.0(4) . . ? C2 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? C3 C4 C6 119.6(4) . . ? C3 C4 C5 119.6(4) . . ? C6 C4 C5 120.8(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C4 118.4(4) . . ? C7 C6 N1 119.9(4) . . ? C4 C6 N1 121.6(4) . . ? C8 C7 C6 120.2(4) . . ? C8 C7 C9 119.6(4) . . ? C6 C7 C9 120.2(4) . . ? C2 C8 C7 122.5(4) . . ? C2 C8 H8A 118.7 . . ? C7 C8 H8A 118.7 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 112.8(3) . . ? N1 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? N1 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C12 C11 N2 110.6(4) . . ? C12 C11 C10 129.4(4) . . ? N2 C11 C10 119.5(4) . . ? C12 C11 Y1 75.5(2) . . ? N2 C11 Y1 72.2(2) . . ? C10 C11 Y1 125.3(3) . . ? C11 C12 C13 106.6(4) . . ? C11 C12 Y1 75.7(2) . . ? C13 C12 Y1 72.6(2) . . ? C11 C12 H12A 126.2 . . ? C13 C12 H12A 126.2 . . ? Y1 C12 H12A 126.2 . . ? C14 C13 C12 107.1(4) . . ? C14 C13 Y1 72.3(2) . . ? C12 C13 Y1 77.8(2) . . ? C14 C13 H13A 125.8 . . ? C12 C13 H13A 125.8 . . ? Y1 C13 H13A 125.8 . . ? C13 C14 N2 110.2(4) . . ? C13 C14 Y1 77.8(3) . . ? N2 C14 Y1 77.2(2) . . ? C13 C14 H14A 124.0 . . ? N2 C14 H14A 124.0 . . ? Y1 C14 H14A 124.0 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? Si1 C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? Si1 C17 H17C 109.5 . . ? Si1 C15' H15D 109.5 . . ? Si1 C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? Si1 C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? Si1 C16' H16D 109.5 . . ? Si1 C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? Si1 C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? Si1 C17' H17D 109.5 . . ? Si1 C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? Si1 C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 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 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.275 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.054 data_ccdc-770561 _database_code_depnum_ccdc_archive 'CCDC 770561' #TrackingRef '- Supporting Information.txt' _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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.5437(8) _cell_length_b 14.8642(9) _cell_length_c 26.9042(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5016.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9968 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.93 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 2.445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.711558 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS-2004/1 - Bruker Nonius area detector scaling and absorption correction' _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 36826 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4922 _reflns_number_gt 3693 _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. The restraints of DFIX, DELU, SIMU and ISOR were used. ; _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^)+(0.0372P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4922 _refine_ls_number_parameters 269 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 1.317 _refine_ls_restrained_S_all 1.342 _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 C18 C 0.827(2) -0.2376(17) 0.6224(8) 0.091(6) Uani 0.49(2) 1 d PDU A 1 H18A H 0.7799 -0.2142 0.5976 0.137 Uiso 0.49(2) 1 calc PR A 1 H18B H 0.7968 -0.2904 0.6372 0.137 Uiso 0.49(2) 1 calc PR A 1 H18C H 0.8943 -0.2528 0.6072 0.137 Uiso 0.49(2) 1 calc PR A 1 C19 C 0.7345(16) -0.1290(12) 0.7054(9) 0.164(9) Uani 0.49(2) 1 d PDU A 1 H19A H 0.7459 -0.0765 0.7254 0.246 Uiso 0.49(2) 1 calc PR A 1 H19B H 0.7186 -0.1794 0.7264 0.246 Uiso 0.49(2) 1 calc PR A 1 H19C H 0.6759 -0.1186 0.6832 0.246 Uiso 0.49(2) 1 calc PR A 1 C20 C 0.9446(18) -0.2118(14) 0.7195(7) 0.160(8) Uani 0.49(2) 1 d PDU A 1 H20A H 1.0093 -0.2298 0.7032 0.240 Uiso 0.49(2) 1 calc PR A 1 H20B H 0.9095 -0.2639 0.7328 0.240 Uiso 0.49(2) 1 calc PR A 1 H20C H 0.9612 -0.1708 0.7460 0.240 Uiso 0.49(2) 1 calc PR A 1 C18' C 0.850(2) -0.2472(17) 0.6270(9) 0.109(8) Uani 0.51(2) 1 d PDU A 2 H18D H 0.8382 -0.2254 0.5939 0.163 Uiso 0.51(2) 1 calc PR A 2 H18E H 0.7940 -0.2885 0.6357 0.163 Uiso 0.51(2) 1 calc PR A 2 H18F H 0.9173 -0.2775 0.6286 0.163 Uiso 0.51(2) 1 calc PR A 2 C19' C 0.6970(8) -0.1124(10) 0.6691(7) 0.122(5) Uani 0.51(2) 1 d PDU A 2 H19D H 0.6916 -0.0520 0.6815 0.183 Uiso 0.51(2) 1 calc PR A 2 H19E H 0.6550 -0.1518 0.6895 0.183 Uiso 0.51(2) 1 calc PR A 2 H19F H 0.6713 -0.1145 0.6356 0.183 Uiso 0.51(2) 1 calc PR A 2 C20' C 0.8692(19) -0.1890(13) 0.7331(4) 0.156(7) Uani 0.51(2) 1 d PDU A 2 H20D H 0.8595 -0.1394 0.7555 0.234 Uiso 0.51(2) 1 calc PR A 2 H20E H 0.9402 -0.2122 0.7366 0.234 Uiso 0.51(2) 1 calc PR A 2 H20F H 0.8186 -0.2354 0.7408 0.234 Uiso 0.51(2) 1 calc PR A 2 Sm1 Sm 0.961755(13) -0.062009(13) 0.565649(7) 0.05411(9) Uani 1 1 d . . . Si1 Si 0.96031(10) 0.03147(10) 0.67778(5) 0.0844(4) Uani 1 1 d . . . Si2 Si 0.84949(14) -0.15172(10) 0.67088(5) 0.1113(5) Uani 1 1 d D . . N1 N 0.9354(2) 0.1740(2) 0.46153(11) 0.0585(7) Uani 1 1 d . . . N2 N 0.8809(2) -0.0029(2) 0.47593(11) 0.0593(7) Uani 1 1 d . . . N3 N 0.9227(3) -0.0649(2) 0.64783(12) 0.0740(9) Uani 1 1 d . A . C1 C 0.9094(6) 0.5205(3) 0.3687(2) 0.131(2) Uani 1 1 d . . . H1A H 0.8663 0.5169 0.3392 0.197 Uiso 1 1 calc R . . H1B H 0.9806 0.5378 0.3597 0.197 Uiso 1 1 calc R . . H1C H 0.8798 0.5645 0.3908 0.197 Uiso 1 1 calc R . . C2 C 0.9117(4) 0.4299(3) 0.39408(19) 0.0832(13) Uani 1 1 d . . . C3 C 0.9691(3) 0.4182(3) 0.43760(16) 0.0743(13) Uani 1 1 d . . . H3A H 1.0041 0.4674 0.4514 0.089 Uiso 1 1 calc R . . C4 C 0.9760(3) 0.3361(2) 0.46105(15) 0.0616(9) Uani 1 1 d . . . C5 C 1.0418(3) 0.3273(3) 0.50800(17) 0.0846(13) Uani 1 1 d . . . H5A H 1.0711 0.3849 0.5166 0.127 Uiso 1 1 calc R . . H5B H 1.0986 0.2852 0.5025 0.127 Uiso 1 1 calc R . . H5C H 0.9973 0.3062 0.5346 0.127 Uiso 1 1 calc R . . C6 C 0.9241(3) 0.2611(3) 0.44065(13) 0.0585(9) Uani 1 1 d . . . C7 C 0.8637(3) 0.2736(3) 0.39796(15) 0.0736(11) Uani 1 1 d . . . C8 C 0.8053(4) 0.1938(3) 0.37461(19) 0.1158(18) Uani 1 1 d . . . H8A H 0.8161 0.1412 0.3947 0.174 Uiso 1 1 calc R . . H8B H 0.8326 0.1833 0.3418 0.174 Uiso 1 1 calc R . . H8C H 0.7304 0.2068 0.3727 0.174 Uiso 1 1 calc R . . C9 C 0.8596(3) 0.3568(3) 0.37564(17) 0.0875(13) Uani 1 1 d . . . H9A H 0.8196 0.3634 0.3468 0.105 Uiso 1 1 calc R . . C10 C 0.8605(3) 0.1571(3) 0.50167(16) 0.0775(11) Uani 1 1 d . . . H10A H 0.7946 0.1889 0.4949 0.093 Uiso 1 1 calc R . . H10B H 0.8898 0.1807 0.5324 0.093 Uiso 1 1 calc R . . C11 C 0.8370(3) 0.0595(3) 0.50815(15) 0.0631(9) Uani 1 1 d . . . C12 C 0.7631(3) 0.0175(3) 0.53874(17) 0.0793(12) Uani 1 1 d . . . H12A H 0.7137 0.0479 0.5614 0.095 Uiso 1 1 calc R . . C13 C 0.7589(3) -0.0725(3) 0.52485(18) 0.0860(14) Uani 1 1 d . . . H13A H 0.7033 -0.1155 0.5345 0.103 Uiso 1 1 calc R . . C14 C 0.8298(3) -0.0834(3) 0.48678(16) 0.0732(11) Uani 1 1 d . . . H14A H 0.8310 -0.1361 0.4649 0.088 Uiso 1 1 calc R . . C15 C 0.8511(5) 0.0901(4) 0.7109(2) 0.137(2) Uani 1 1 d . . . H15A H 0.8761 0.1099 0.7428 0.205 Uiso 1 1 calc R . . H15B H 0.7922 0.0496 0.7153 0.205 Uiso 1 1 calc R . . H15C H 0.8284 0.1412 0.6918 0.205 Uiso 1 1 calc R . . C16 C 1.0700(6) 0.0129(6) 0.7223(2) 0.170(3) Uani 1 1 d . . . H16A H 1.0556 0.0452 0.7524 0.255 Uiso 1 1 calc R . . H16B H 1.1356 0.0341 0.7081 0.255 Uiso 1 1 calc R . . H16C H 1.0759 -0.0501 0.7294 0.255 Uiso 1 1 calc R . . C17 C 1.0114(5) 0.1106(4) 0.6299(2) 0.133(2) Uani 1 1 d . . . H17A H 1.0297 0.1667 0.6453 0.199 Uiso 1 1 calc R . . H17B H 0.9574 0.1205 0.6052 0.199 Uiso 1 1 calc R . . H17C H 1.0735 0.0853 0.6144 0.199 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 C18 0.098(12) 0.089(10) 0.086(9) 0.010(8) 0.023(7) 0.013(9) C19 0.185(14) 0.163(13) 0.145(14) -0.019(11) 0.100(12) 0.002(10) C20 0.208(16) 0.156(13) 0.116(11) 0.066(10) -0.004(10) -0.020(11) C18' 0.097(12) 0.098(13) 0.130(14) -0.014(11) 0.037(9) -0.020(9) C19' 0.100(8) 0.140(10) 0.127(11) -0.023(9) 0.052(7) -0.015(7) C20' 0.214(16) 0.164(12) 0.089(8) 0.027(8) 0.022(9) -0.026(12) Sm1 0.05051(12) 0.05649(14) 0.05533(14) 0.00152(8) -0.00085(8) -0.00075(8) Si1 0.1008(10) 0.0896(9) 0.0628(7) -0.0069(7) -0.0112(6) 0.0142(7) Si2 0.1577(14) 0.0951(10) 0.0813(9) -0.0018(8) 0.0497(9) -0.0115(9) N1 0.0530(15) 0.0550(18) 0.0676(19) 0.0023(15) 0.0035(14) 0.0012(13) N2 0.0522(15) 0.0614(19) 0.0644(18) 0.0063(15) -0.0114(13) -0.0080(15) N3 0.085(2) 0.081(2) 0.0562(19) 0.0000(16) 0.0046(17) 0.0072(17) C1 0.184(6) 0.072(3) 0.138(5) 0.025(3) 0.025(5) 0.030(4) C2 0.091(3) 0.069(3) 0.090(3) 0.009(2) 0.021(3) 0.022(2) C3 0.074(3) 0.054(2) 0.095(4) -0.005(2) 0.019(2) 0.0019(18) C4 0.053(2) 0.053(2) 0.079(3) -0.0049(19) 0.0124(18) 0.0021(16) C5 0.081(3) 0.073(3) 0.101(3) -0.011(3) -0.009(2) -0.003(2) C6 0.0484(17) 0.059(2) 0.068(2) -0.0018(18) 0.0072(16) 0.0034(17) C7 0.072(3) 0.069(3) 0.080(3) 0.000(2) -0.009(2) 0.004(2) C8 0.119(4) 0.107(4) 0.121(4) 0.002(3) -0.054(3) -0.015(3) C9 0.094(3) 0.084(3) 0.085(3) 0.007(3) -0.005(2) 0.019(3) C10 0.070(2) 0.071(3) 0.092(3) 0.010(2) 0.016(2) 0.012(2) C11 0.0461(18) 0.069(2) 0.074(2) 0.010(2) 0.0004(17) 0.0074(18) C12 0.046(2) 0.093(3) 0.098(3) 0.026(3) 0.006(2) 0.004(2) C13 0.054(2) 0.106(4) 0.099(3) 0.034(3) -0.008(2) -0.026(2) C14 0.068(2) 0.070(3) 0.081(3) 0.011(2) -0.027(2) -0.020(2) C15 0.171(6) 0.102(4) 0.137(5) -0.031(4) 0.029(4) 0.025(4) C16 0.193(7) 0.166(7) 0.150(6) -0.027(5) -0.094(6) 0.034(6) C17 0.189(6) 0.102(4) 0.107(4) -0.014(4) 0.001(4) -0.052(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 C18 Si2 1.845(14) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 Si2 1.747(11) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 Si2 1.983(12) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C18' Si2 1.846(13) . ? C18' H18D 0.9600 . ? C18' H18E 0.9600 . ? C18' H18F 0.9600 . ? C19' Si2 2.000(11) . ? C19' H19D 0.9600 . ? C19' H19E 0.9600 . ? C19' H19F 0.9600 . ? C20' Si2 1.781(11) . ? C20' H20D 0.9600 . ? C20' H20E 0.9600 . ? C20' H20F 0.9600 . ? Sm1 N1 2.229(3) 5_756 ? Sm1 N3 2.265(3) . ? Sm1 N2 2.465(3) 5_756 ? Sm1 C14 2.710(4) . ? Sm1 N2 2.762(3) . ? Sm1 C13 2.776(4) . ? Sm1 C11 2.847(4) . ? Sm1 C12 2.852(4) . ? Si1 N3 1.709(4) . ? Si1 C16 1.845(6) . ? Si1 C15 1.852(5) . ? Si1 C17 1.859(6) . ? Si2 N3 1.701(4) . ? N1 C6 1.418(4) . ? N1 C10 1.453(4) . ? N1 Sm1 2.229(3) 5_756 ? N2 C11 1.384(5) . ? N2 C14 1.388(5) . ? N2 Sm1 2.465(3) 5_756 ? C1 C2 1.512(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C9 1.361(6) . ? C2 C3 1.385(6) . ? C3 C4 1.377(6) . ? C3 H3A 0.9300 . ? C4 C6 1.403(5) . ? C4 C5 1.515(5) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.388(5) . ? C7 C9 1.375(6) . ? C7 C8 1.530(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9300 . ? C10 C11 1.490(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.388(5) . ? C12 C13 1.391(6) . ? C12 H12A 0.9800 . ? C13 C14 1.366(6) . ? C13 H13A 0.9800 . ? C14 H14A 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 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 Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? Si2 C18' H18D 109.5 . . ? Si2 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? Si2 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? Si2 C19' H19D 109.5 . . ? Si2 C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? Si2 C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? Si2 C20' H20D 109.5 . . ? Si2 C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? Si2 C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? N1 Sm1 N3 115.56(11) 5_756 . ? N1 Sm1 N2 71.35(10) 5_756 5_756 ? N3 Sm1 N2 128.56(11) . 5_756 ? N1 Sm1 C14 90.53(13) 5_756 . ? N3 Sm1 C14 129.05(13) . . ? N2 Sm1 C14 100.35(11) 5_756 . ? N1 Sm1 N2 99.40(10) 5_756 . ? N3 Sm1 N2 141.24(11) . . ? N2 Sm1 N2 76.87(9) 5_756 . ? C14 Sm1 N2 29.37(10) . . ? N1 Sm1 C13 111.03(14) 5_756 . ? N3 Sm1 C13 100.75(14) . . ? N2 Sm1 C13 125.21(11) 5_756 . ? C14 Sm1 C13 28.81(13) . . ? N2 Sm1 C13 48.37(10) . . ? N1 Sm1 C11 127.85(11) 5_756 . ? N3 Sm1 C11 115.05(12) . . ? N2 Sm1 C11 86.85(9) 5_756 . ? C14 Sm1 C11 46.61(11) . . ? N2 Sm1 C11 28.52(10) . . ? C13 Sm1 C11 46.92(12) . . ? N1 Sm1 C12 137.06(13) 5_756 . ? N3 Sm1 C12 93.82(13) . . ? N2 Sm1 C12 114.96(11) 5_756 . ? C14 Sm1 C12 46.84(14) . . ? N2 Sm1 C12 47.57(11) . . ? C13 Sm1 C12 28.58(12) . . ? C11 Sm1 C12 28.19(11) . . ? N1 Sm1 Sm1 85.27(8) 5_756 5_756 ? N3 Sm1 Sm1 154.21(8) . 5_756 ? N2 Sm1 Sm1 41.01(6) 5_756 5_756 ? C14 Sm1 Sm1 61.37(9) . 5_756 ? N2 Sm1 Sm1 35.86(6) . 5_756 ? C13 Sm1 Sm1 84.21(9) . 5_756 ? C11 Sm1 Sm1 51.31(7) . 5_756 ? C12 Sm1 Sm1 78.42(8) . 5_756 ? N3 Si1 C16 112.8(3) . . ? N3 Si1 C15 114.6(2) . . ? C16 Si1 C15 108.0(3) . . ? N3 Si1 C17 107.4(2) . . ? C16 Si1 C17 106.7(3) . . ? C15 Si1 C17 106.9(3) . . ? N3 Si2 C19 119.5(6) . . ? N3 Si2 C20' 120.2(7) . . ? C19 Si2 C20' 71.1(7) . . ? N3 Si2 C18 110.4(10) . . ? C19 Si2 C18 112.7(11) . . ? C20' Si2 C18 118.0(12) . . ? N3 Si2 C18' 110.5(10) . . ? C19 Si2 C18' 119.3(12) . . ? C20' Si2 C18' 111.2(10) . . ? C18 Si2 C18' 10.5(15) . . ? N3 Si2 C20 104.9(6) . . ? C19 Si2 C20 103.5(7) . . ? C20' Si2 C20 32.5(5) . . ? C18 Si2 C20 104.2(10) . . ? C18' Si2 C20 94.2(11) . . ? N3 Si2 C19' 106.6(5) . . ? C19 Si2 C19' 33.6(6) . . ? C20' Si2 C19' 104.2(6) . . ? C18 Si2 C19' 92.4(10) . . ? C18' Si2 C19' 102.2(9) . . ? C20 Si2 C19' 136.3(6) . . ? C6 N1 C10 112.8(3) . . ? C6 N1 Sm1 127.5(2) . 5_756 ? C10 N1 Sm1 119.3(2) . 5_756 ? C11 N2 C14 105.2(3) . . ? C11 N2 Sm1 109.9(2) . 5_756 ? C14 N2 Sm1 143.4(3) . 5_756 ? C11 N2 Sm1 79.15(19) . . ? C14 N2 Sm1 73.25(19) . . ? Sm1 N2 Sm1 103.13(9) 5_756 . ? Si2 N3 Si1 127.8(2) . . ? Si2 N3 Sm1 119.12(17) . . ? Si1 N3 Sm1 112.63(17) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C9 C2 C3 117.3(4) . . ? C9 C2 C1 122.5(5) . . ? C3 C2 C1 120.2(5) . . ? C4 C3 C2 122.0(4) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C3 C4 C6 119.8(4) . . ? C3 C4 C5 119.5(4) . . ? C6 C4 C5 120.7(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C4 118.0(4) . . ? C7 C6 N1 120.3(3) . . ? C4 C6 N1 121.6(3) . . ? C9 C7 C6 120.1(4) . . ? C9 C7 C8 120.0(4) . . ? C6 C7 C8 119.8(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C2 C9 C7 122.7(4) . . ? C2 C9 H9A 118.6 . . ? C7 C9 H9A 118.6 . . ? N1 C10 C11 112.5(3) . . ? N1 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? N1 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? N2 C11 C12 109.6(4) . . ? N2 C11 C10 120.0(3) . . ? C12 C11 C10 129.7(4) . . ? N2 C11 Sm1 72.32(18) . . ? C12 C11 Sm1 76.1(2) . . ? C10 C11 Sm1 124.9(3) . . ? C11 C12 C13 107.4(4) . . ? C11 C12 Sm1 75.7(2) . . ? C13 C12 Sm1 72.7(2) . . ? C11 C12 H12A 125.8 . . ? C13 C12 H12A 125.8 . . ? Sm1 C12 H12A 125.8 . . ? C14 C13 C12 106.9(4) . . ? C14 C13 Sm1 72.9(2) . . ? C12 C13 Sm1 78.7(2) . . ? C14 C13 H13A 125.7 . . ? C12 C13 H13A 125.7 . . ? Sm1 C13 H13A 125.7 . . ? C13 C14 N2 110.9(4) . . ? C13 C14 Sm1 78.3(2) . . ? N2 C14 Sm1 77.37(19) . . ? C13 C14 H14A 123.7 . . ? N2 C14 H14A 123.7 . . ? Sm1 C14 H14A 123.7 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.471 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.061 data_ccdc-770562 _database_code_depnum_ccdc_archive 'CCDC 770562' #TrackingRef '- Supporting Information.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H68 Er2 N6 Si4' _chemical_formula_weight 1079.88 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.4386(8) _cell_length_b 14.9104(10) _cell_length_c 26.6642(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4945.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9984 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.56 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 3.499 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.647869 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS-2004/1 - Bruker Nonius area detector scaling and absorption correction' _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 40636 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.63 _reflns_number_total 5739 _reflns_number_gt 3912 _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. The restraints of DFIX, DELU, SIMU and ISOR were used. ; _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^)+(0.0347P)^2^+0.6813P] 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 5739 _refine_ls_number_parameters 269 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.237 _refine_ls_restrained_S_all 1.249 _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 C15 C 0.564(2) -0.213(2) 0.2158(10) 0.148(10) Uani 0.38(2) 1 d PDU A 1 H15A H 0.5492 -0.1737 0.2434 0.222 Uiso 0.38(2) 1 calc PR A 1 H15B H 0.5992 -0.2661 0.2279 0.222 Uiso 0.38(2) 1 calc PR A 1 H15C H 0.4974 -0.2296 0.1999 0.222 Uiso 0.38(2) 1 calc PR A 1 C16 C 0.773(2) -0.1268(16) 0.2016(12) 0.137(10) Uani 0.38(2) 1 d PDU A 1 H16A H 0.7615 -0.0734 0.2210 0.206 Uiso 0.38(2) 1 calc PR A 1 H16B H 0.8322 -0.1176 0.1790 0.206 Uiso 0.38(2) 1 calc PR A 1 H16C H 0.7894 -0.1758 0.2238 0.206 Uiso 0.38(2) 1 calc PR A 1 C17 C 0.680(3) -0.235(2) 0.1169(10) 0.084(8) Uani 0.38(2) 1 d PDU A 1 H17A H 0.6690 -0.2069 0.0848 0.126 Uiso 0.38(2) 1 calc PR A 1 H17B H 0.6297 -0.2837 0.1206 0.126 Uiso 0.38(2) 1 calc PR A 1 H17C H 0.7517 -0.2574 0.1191 0.126 Uiso 0.38(2) 1 calc PR A 1 C15' C 0.631(2) -0.1861(13) 0.2305(4) 0.152(7) Uani 0.62(2) 1 d PDU A 2 H15D H 0.6327 -0.1346 0.2521 0.227 Uiso 0.62(2) 1 calc PR A 2 H15E H 0.6848 -0.2283 0.2409 0.227 Uiso 0.62(2) 1 calc PR A 2 H15F H 0.5613 -0.2138 0.2324 0.227 Uiso 0.62(2) 1 calc PR A 2 C16' C 0.8055(9) -0.1099(11) 0.1664(8) 0.129(6) Uani 0.62(2) 1 d PDU A 2 H16D H 0.8096 -0.0522 0.1823 0.193 Uiso 0.62(2) 1 calc PR A 2 H16E H 0.8299 -0.1052 0.1324 0.193 Uiso 0.62(2) 1 calc PR A 2 H16F H 0.8500 -0.1517 0.1843 0.193 Uiso 0.62(2) 1 calc PR A 2 C17' C 0.6604(18) -0.2493(14) 0.1243(8) 0.097(6) Uani 0.62(2) 1 d PDU A 2 H17D H 0.5883 -0.2672 0.1162 0.145 Uiso 0.62(2) 1 calc PR A 2 H17E H 0.6971 -0.2982 0.1403 0.145 Uiso 0.62(2) 1 calc PR A 2 H17F H 0.6977 -0.2332 0.0941 0.145 Uiso 0.62(2) 1 calc PR A 2 Er1 Er 0.539996(14) -0.061410(13) 0.063595(7) 0.05142(8) Uani 1 1 d . . . N1 N 0.5594(3) 0.1730(2) -0.04021(14) 0.0548(9) Uani 1 1 d . . . N2 N 0.6134(3) -0.0036(2) -0.02553(14) 0.0572(9) Uani 1 1 d . . . N3 N 0.5793(4) -0.0665(3) 0.14354(15) 0.0726(11) Uani 1 1 d . A . Si1 Si 0.65661(17) -0.15193(13) 0.16718(6) 0.1058(6) Uani 1 1 d D . . Si2 Si 0.54217(13) 0.02800(12) 0.17593(6) 0.0829(5) Uani 1 1 d . . . C1 C 0.5948(7) 0.5219(4) -0.1305(3) 0.121(2) Uani 1 1 d . . . H1A H 0.6380 0.5185 -0.1603 0.182 Uiso 1 1 calc R . . H1B H 0.6266 0.5638 -0.1075 0.182 Uiso 1 1 calc R . . H1C H 0.5237 0.5416 -0.1391 0.182 Uiso 1 1 calc R . . C2 C 0.5889(5) 0.4308(3) -0.1063(2) 0.0786(15) Uani 1 1 d . . . C3 C 0.6401(4) 0.3572(4) -0.1255(2) 0.0795(15) Uani 1 1 d . . . H3A H 0.6814 0.3641 -0.1543 0.095 Uiso 1 1 calc R . . C4 C 0.6332(4) 0.2731(3) -0.10396(19) 0.0703(13) Uani 1 1 d . . . C5 C 0.6921(5) 0.1947(4) -0.1279(2) 0.112(2) Uani 1 1 d . . . H5A H 0.6783 0.1411 -0.1090 0.167 Uiso 1 1 calc R . . H5B H 0.7680 0.2066 -0.1281 0.167 Uiso 1 1 calc R . . H5C H 0.6673 0.1868 -0.1617 0.167 Uiso 1 1 calc R . . C6 C 0.5726(3) 0.2605(3) -0.06079(17) 0.0569(11) Uani 1 1 d . . . C7 C 0.5221(3) 0.3355(3) -0.03936(18) 0.0586(11) Uani 1 1 d . . . C8 C 0.4564(4) 0.3270(3) 0.0079(2) 0.0773(15) Uani 1 1 d . . . H8A H 0.4292 0.3849 0.0173 0.116 Uiso 1 1 calc R . . H8B H 0.5008 0.3040 0.0344 0.116 Uiso 1 1 calc R . . H8C H 0.3974 0.2868 0.0022 0.116 Uiso 1 1 calc R . . C9 C 0.5306(4) 0.4188(3) -0.0625(2) 0.0711(15) Uani 1 1 d . . . H9A H 0.4963 0.4679 -0.0481 0.085 Uiso 1 1 calc R . . C10 C 0.6355(4) 0.1565(3) 0.00037(19) 0.0735(14) Uani 1 1 d . . . H10A H 0.6066 0.1803 0.0314 0.088 Uiso 1 1 calc R . . H10B H 0.7022 0.1877 -0.0067 0.088 Uiso 1 1 calc R . . C11 C 0.6582(3) 0.0582(3) 0.00682(18) 0.0592(11) Uani 1 1 d . . . C12 C 0.7332(4) 0.0164(4) 0.0378(2) 0.0723(14) Uani 1 1 d . . . H12A H 0.7831 0.0465 0.0607 0.087 Uiso 1 1 calc R . . C13 C 0.7372(4) -0.0736(4) 0.0233(2) 0.0812(16) Uani 1 1 d . . . H13A H 0.7929 -0.1168 0.0330 0.097 Uiso 1 1 calc R . . C14 C 0.6646(4) -0.0840(3) -0.0154(2) 0.0693(14) Uani 1 1 d . . . H14A H 0.6619 -0.1366 -0.0375 0.083 Uiso 1 1 calc R . . C18 C 0.4319(7) 0.0060(6) 0.2196(3) 0.163(4) Uani 1 1 d . A . H18A H 0.4451 0.0369 0.2506 0.245 Uiso 1 1 calc R . . H18B H 0.4271 -0.0573 0.2259 0.245 Uiso 1 1 calc R . . H18C H 0.3656 0.0268 0.2053 0.245 Uiso 1 1 calc R . . C19 C 0.4897(6) 0.1098(5) 0.1302(3) 0.132(3) Uani 1 1 d . A . H19A H 0.4710 0.1643 0.1472 0.197 Uiso 1 1 calc R . . H19B H 0.4270 0.0855 0.1141 0.197 Uiso 1 1 calc R . . H19C H 0.5437 0.1221 0.1054 0.197 Uiso 1 1 calc R . . C20 C 0.6525(6) 0.0844(4) 0.2106(3) 0.134(3) Uani 1 1 d . A . H20A H 0.6268 0.1035 0.2428 0.201 Uiso 1 1 calc R . . H20B H 0.6768 0.1355 0.1919 0.201 Uiso 1 1 calc R . . H20C H 0.7111 0.0432 0.2150 0.201 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 C15 0.173(18) 0.156(16) 0.115(15) 0.035(13) -0.006(13) 0.018(14) C16 0.165(16) 0.127(14) 0.121(16) -0.001(12) -0.084(14) 0.013(12) C17 0.090(14) 0.091(13) 0.072(12) 0.006(10) -0.005(10) -0.014(11) C15' 0.215(16) 0.165(12) 0.075(7) 0.020(8) -0.023(9) 0.039(12) C16' 0.106(9) 0.154(10) 0.126(12) -0.027(10) -0.056(8) 0.008(8) C17' 0.082(10) 0.097(10) 0.110(12) -0.012(9) -0.033(9) 0.010(8) Er1 0.04591(12) 0.05846(13) 0.04990(13) 0.00173(9) 0.00042(9) -0.00006(9) N1 0.050(2) 0.056(2) 0.059(2) 0.0011(17) -0.0046(17) -0.0017(16) N2 0.047(2) 0.063(2) 0.061(2) 0.0043(18) 0.0088(18) 0.0066(18) N3 0.073(3) 0.091(3) 0.054(2) -0.004(2) -0.004(2) -0.010(2) Si1 0.1347(16) 0.1112(13) 0.0715(11) -0.0044(9) -0.0413(11) 0.0159(12) Si2 0.0953(13) 0.0971(11) 0.0565(9) -0.0064(8) 0.0087(8) -0.0131(9) C1 0.167(7) 0.075(4) 0.122(6) 0.027(4) -0.015(5) -0.031(4) C2 0.083(4) 0.067(3) 0.086(4) 0.010(3) -0.019(3) -0.020(3) C3 0.084(4) 0.080(3) 0.074(4) 0.008(3) 0.011(3) -0.016(3) C4 0.066(3) 0.072(3) 0.073(3) 0.002(3) 0.009(3) 0.000(3) C5 0.117(5) 0.096(4) 0.122(5) 0.010(4) 0.062(4) 0.015(4) C6 0.046(2) 0.063(3) 0.061(3) 0.000(2) -0.005(2) -0.005(2) C7 0.051(3) 0.056(3) 0.069(3) -0.005(2) -0.009(2) -0.005(2) C8 0.076(4) 0.067(3) 0.089(4) -0.007(3) 0.010(3) 0.004(3) C9 0.072(4) 0.054(3) 0.088(4) -0.010(2) -0.017(3) -0.004(2) C10 0.065(3) 0.073(3) 0.082(3) 0.009(3) -0.018(3) -0.012(3) C11 0.040(2) 0.070(3) 0.067(3) 0.011(2) 0.000(2) -0.003(2) C12 0.043(3) 0.092(4) 0.082(4) 0.022(3) -0.004(2) -0.004(3) C13 0.048(3) 0.098(4) 0.098(4) 0.031(3) 0.009(3) 0.021(3) C14 0.060(3) 0.071(3) 0.077(3) 0.009(2) 0.023(3) 0.017(2) C18 0.187(8) 0.156(7) 0.147(8) -0.036(6) 0.096(7) -0.037(7) C19 0.172(7) 0.118(6) 0.105(5) -0.010(5) -0.004(5) 0.054(5) C20 0.163(8) 0.107(5) 0.133(6) -0.030(4) -0.045(6) -0.017(5) _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 C15 Si1 1.961(15) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 Si1 1.756(13) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 Si1 1.847(16) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C15' Si1 1.793(10) . ? C15' H15D 0.9600 . ? C15' H15E 0.9600 . ? C15' H15F 0.9600 . ? C16' Si1 1.955(11) . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17' Si1 1.849(11) . ? C17' H17D 0.9600 . ? C17' H17E 0.9600 . ? C17' H17F 0.9600 . ? Er1 N1 2.164(3) 5_655 ? Er1 N3 2.189(4) . ? Er1 N2 2.368(3) 5_655 ? Er1 C14 2.638(5) . ? Er1 C13 2.684(5) . ? Er1 N2 2.688(3) . ? Er1 C12 2.756(5) . ? Er1 C11 2.763(4) . ? N1 C6 1.426(5) . ? N1 C10 1.459(5) . ? N1 Er1 2.164(3) 5_655 ? N2 C11 1.379(6) . ? N2 C14 1.385(6) . ? N2 Er1 2.368(3) 5_655 ? N3 Si1 1.716(5) . ? N3 Si2 1.716(4) . ? Si2 C18 1.830(7) . ? Si2 C19 1.844(7) . ? Si2 C20 1.856(7) . ? C1 C2 1.505(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.368(7) . ? C2 C9 1.386(7) . ? C3 C4 1.381(6) . ? C3 H3A 0.9300 . ? C4 C6 1.389(6) . ? C4 C5 1.521(7) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.404(6) . ? C7 C9 1.391(6) . ? C7 C8 1.508(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9300 . ? C10 C11 1.503(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.392(6) . ? C12 C13 1.398(7) . ? C12 H12A 0.9800 . ? C13 C14 1.381(7) . ? C13 H13A 0.9800 . ? C14 H14A 0.9800 . ? 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 . ? 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 Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? Si1 C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? Si1 C17 H17C 109.5 . . ? Si1 C15' H15D 109.5 . . ? Si1 C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? Si1 C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? Si1 C16' H16D 109.5 . . ? Si1 C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? Si1 C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? Si1 C17' H17D 109.5 . . ? Si1 C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? Si1 C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? N1 Er1 N3 112.43(14) 5_655 . ? N1 Er1 N2 74.40(12) 5_655 5_655 ? N3 Er1 N2 127.72(15) . 5_655 ? N1 Er1 C14 90.41(16) 5_655 . ? N3 Er1 C14 129.96(17) . . ? N2 Er1 C14 100.57(14) 5_655 . ? N1 Er1 C13 110.75(16) 5_655 . ? N3 Er1 C13 100.55(17) . . ? N2 Er1 C13 126.34(14) 5_655 . ? C14 Er1 C13 30.06(15) . . ? N1 Er1 N2 100.71(13) 5_655 . ? N3 Er1 N2 142.78(14) . . ? N2 Er1 N2 76.32(12) 5_655 . ? C14 Er1 N2 30.13(12) . . ? C13 Er1 N2 50.02(13) . . ? N1 Er1 C12 138.55(16) 5_655 . ? N3 Er1 C12 93.61(16) . . ? N2 Er1 C12 115.03(13) 5_655 . ? C14 Er1 C12 48.83(17) . . ? C13 Er1 C12 29.74(15) . . ? N2 Er1 C12 49.29(13) . . ? N1 Er1 C11 129.95(14) 5_655 . ? N3 Er1 C11 115.92(15) . . ? N2 Er1 C11 85.99(12) 5_655 . ? C14 Er1 C11 48.08(14) . . ? C13 Er1 C11 48.54(14) . . ? N2 Er1 C11 29.27(12) . . ? C12 Er1 C11 29.22(13) . . ? C6 N1 C10 111.4(3) . . ? C6 N1 Er1 131.2(3) . 5_655 ? C10 N1 Er1 117.0(3) . 5_655 ? C11 N2 C14 105.7(4) . . ? C11 N2 Er1 108.7(3) . 5_655 ? C14 N2 Er1 143.9(3) . 5_655 ? C11 N2 Er1 78.4(2) . . ? C14 N2 Er1 72.9(2) . . ? Er1 N2 Er1 103.68(12) 5_655 . ? Si1 N3 Si2 125.1(2) . . ? Si1 N3 Er1 120.6(2) . . ? Si2 N3 Er1 113.7(2) . . ? N3 Si1 C16 119.7(8) . . ? N3 Si1 C15' 117.2(6) . . ? C16 Si1 C15' 73.5(9) . . ? N3 Si1 C17 108.5(14) . . ? C16 Si1 C17 113.3(14) . . ? C15' Si1 C17 121.4(14) . . ? N3 Si1 C17' 111.7(8) . . ? C16 Si1 C17' 118.0(13) . . ? C15' Si1 C17' 111.3(9) . . ? C17 Si1 C17' 11.7(16) . . ? N3 Si1 C16' 106.8(6) . . ? C16 Si1 C16' 32.4(8) . . ? C15' Si1 C16' 105.7(6) . . ? C17 Si1 C16' 93.5(12) . . ? C17' Si1 C16' 102.8(8) . . ? N3 Si1 C15 105.0(9) . . ? C16 Si1 C15 103.8(9) . . ? C15' Si1 C15 30.7(7) . . ? C17 Si1 C15 105.0(12) . . ? C17' Si1 C15 93.4(12) . . ? C16' Si1 C15 135.5(8) . . ? N3 Si2 C18 112.0(3) . . ? N3 Si2 C19 107.8(3) . . ? C18 Si2 C19 105.9(4) . . ? N3 Si2 C20 115.0(3) . . ? C18 Si2 C20 108.6(4) . . ? C19 Si2 C20 107.0(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C9 117.0(5) . . ? C3 C2 C1 122.8(6) . . ? C9 C2 C1 120.2(6) . . ? C2 C3 C4 123.0(5) . . ? C2 C3 H3A 118.5 . . ? C4 C3 H3A 118.5 . . ? C3 C4 C6 120.0(5) . . ? C3 C4 C5 119.6(5) . . ? C6 C4 C5 120.4(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 C7 118.2(4) . . ? C4 C6 N1 120.4(4) . . ? C7 C6 N1 121.3(4) . . ? C9 C7 C6 119.7(5) . . ? C9 C7 C8 119.1(4) . . ? C6 C7 C8 121.1(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C2 C9 C7 121.9(5) . . ? C2 C9 H9A 119.0 . . ? C7 C9 H9A 119.0 . . ? N1 C10 C11 111.8(4) . . ? N1 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N1 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? N2 C11 C12 110.1(4) . . ? N2 C11 C10 120.2(4) . . ? C12 C11 C10 129.1(5) . . ? N2 C11 Er1 72.4(2) . . ? C12 C11 Er1 75.1(3) . . ? C10 C11 Er1 126.3(3) . . ? C11 C12 C13 106.9(5) . . ? C11 C12 Er1 75.7(3) . . ? C13 C12 Er1 72.3(3) . . ? C11 C12 H12A 126.1 . . ? C13 C12 H12A 126.1 . . ? Er1 C12 H12A 126.1 . . ? C14 C13 C12 106.9(4) . . ? C14 C13 Er1 73.1(3) . . ? C12 C13 Er1 78.0(3) . . ? C14 C13 H13A 125.8 . . ? C12 C13 H13A 125.8 . . ? Er1 C13 H13A 125.8 . . ? C13 C14 N2 110.4(5) . . ? C13 C14 Er1 76.8(3) . . ? N2 C14 Er1 76.9(2) . . ? C13 C14 H14A 124.1 . . ? N2 C14 H14A 124.1 . . ? Er1 C14 H14A 124.1 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 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 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.865 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.079