# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email hroesky@gwdg.de _publ_contact_author_name 'Herbert W. Roesky' _publ_author_name H.Roesky data_p21c _database_code_depnum_ccdc_archive 'CCDC 817514' #TrackingRef '4672_web_deposit_cif_file_0_JakobHey_1300200439.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H52 N4 O4 Si' _chemical_formula_sum 'C35 H52 N4 O4 Si' _chemical_formula_weight 620.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2681(14) _cell_length_b 12.0341(12) _cell_length_c 21.837(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.780(5) _cell_angle_gamma 90.00 _cell_volume 3474.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8587 _cell_measurement_theta_min 2.2665 _cell_measurement_theta_max 17.382 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9371 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS 2008/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.56086 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'INCOATEC Ag I\mS microfocus source' _diffrn_radiation_monochromator 'INCOATEC mirror optics' _diffrn_measurement_device_type 'Bruker APEX II Quazar' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 97129 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 21.06 _reflns_number_total 7620 _reflns_number_gt 6297 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2008.11' _computing_cell_refinement 'SAINT V7.68A' _computing_data_reduction 'SAINT V7.46A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XSHELL v4.01' _computing_publication_material 'XSHELL v4.01' _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. Disorder of one Ethoxy group was described. Coordinates for H atom H1S located at Silicon atomm Si1 was freely refined with Ueq set to 1.5 times the Ueq of Si1. Checkcif "222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) 4.27 Ratio" is due to this approach. Checkcif "220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) 3.93 Ratio" is due to rather large Ueq of neighboring isopropyl methyl groups which could not be refined as disordered groups. ; _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^)+(0.0485P)^2^+1.9805P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7620 _refine_ls_number_parameters 440 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.100 _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 C1 C 0.38862(12) -0.01566(14) 0.31918(8) 0.0181(3) Uani 1 1 d . . . N1 N 0.32331(11) -0.00897(12) 0.27325(7) 0.0202(3) Uani 1 1 d . . . O1 O 0.39167(8) 0.05641(9) 0.36608(5) 0.0183(2) Uani 1 1 d . . . Si1 Si 0.29789(3) 0.15542(4) 0.35888(2) 0.01453(11) Uani 1 1 d . . . H1S H 0.2849(14) 0.2560(16) 0.3299(8) 0.022 Uiso 1 1 d . . . C2 C 0.46570(16) -0.17121(17) 0.27670(9) 0.0331(5) Uani 1 1 d . . . H2A H 0.4620 -0.1314 0.2369 0.040 Uiso 1 1 calc R . . H2B H 0.4078 -0.2232 0.2763 0.040 Uiso 1 1 calc R . . N2 N 0.25985(10) 0.08213(11) 0.28666(6) 0.0174(3) Uani 1 1 d . A . O2 O 0.46194(9) -0.09251(10) 0.32683(6) 0.0231(3) Uani 1 1 d . . . C3 C 0.56276(16) -0.23373(17) 0.28605(9) 0.0331(5) Uani 1 1 d . . . H3A H 0.6196 -0.1823 0.2836 0.050 Uiso 1 1 calc R . . H3B H 0.5650 -0.2907 0.2542 0.050 Uiso 1 1 calc R . . H3C H 0.5675 -0.2692 0.3266 0.050 Uiso 1 1 calc R . . N3 N 0.19738(10) 0.11477(11) 0.40526(6) 0.0149(3) Uani 1 1 d . . . O3 O 0.14199(9) 0.20457(11) 0.24790(6) 0.0264(3) Uani 1 1 d . A . C4 C 0.19700(13) 0.12508(15) 0.24072(8) 0.0221(4) Uani 1 1 d D . . N4 N 0.37583(10) 0.23036(11) 0.42493(6) 0.0145(3) Uani 1 1 d . . . O4 O 0.1966(5) 0.0607(4) 0.1880(2) 0.0193(9) Uani 0.644(5) 1 d PD A 1 C5 C 0.1290(3) 0.1032(3) 0.1377(2) 0.0198(9) Uani 0.644(5) 1 d PD A 1 H5A H 0.0658 0.1298 0.1540 0.024 Uiso 0.644(5) 1 calc PR A 1 H5B H 0.1112 0.0426 0.1081 0.024 Uiso 0.644(5) 1 calc PR A 1 C6 C 0.1773(2) 0.1974(3) 0.10512(15) 0.0291(9) Uani 0.644(5) 1 d PD A 1 H6A H 0.1298 0.2250 0.0718 0.044 Uiso 0.644(5) 1 calc PR A 1 H6B H 0.2389 0.1707 0.0880 0.044 Uiso 0.644(5) 1 calc PR A 1 H6C H 0.1946 0.2576 0.1343 0.044 Uiso 0.644(5) 1 calc PR A 1 O4' O 0.2082(9) 0.0941(7) 0.1832(4) 0.0254(19) Uani 0.356(5) 1 d PD A 2 C5' C 0.1428(7) 0.1478(7) 0.1356(4) 0.0273(19) Uani 0.356(5) 1 d PD A 2 H5'1 H 0.1551 0.2289 0.1359 0.033 Uiso 0.356(5) 1 calc PR A 2 H5'2 H 0.0709 0.1345 0.1424 0.033 Uiso 0.356(5) 1 calc PR A 2 C6' C 0.1670(5) 0.0990(5) 0.0765(2) 0.0349(17) Uani 0.356(5) 1 d PD A 2 H6'1 H 0.1236 0.1324 0.0430 0.052 Uiso 0.356(5) 1 calc PR A 2 H6'2 H 0.1555 0.0186 0.0772 0.052 Uiso 0.356(5) 1 calc PR A 2 H6'3 H 0.2380 0.1137 0.0702 0.052 Uiso 0.356(5) 1 calc PR A 2 C7 C 0.12320(13) 0.05837(16) 0.50083(8) 0.0232(4) Uani 1 1 d . . . H7S1 H 0.0712 0.1156 0.5034 0.035 Uiso 1 1 calc R . . H7S2 H 0.1485 0.0354 0.5423 0.035 Uiso 1 1 calc R . . H7S3 H 0.0940 -0.0060 0.4782 0.035 Uiso 1 1 calc R . . C8 C 0.20937(12) 0.10472(14) 0.46766(7) 0.0179(3) Uani 1 1 d . . . C9 C 0.29400(13) 0.13944(14) 0.50314(8) 0.0205(4) Uani 1 1 d . . . H9 H 0.3008 0.1154 0.5447 0.025 Uiso 1 1 calc R . . C10 C 0.37146(12) 0.20744(14) 0.48351(8) 0.0182(3) Uani 1 1 d . . . C11 C 0.44440(14) 0.25673(17) 0.53262(8) 0.0275(4) Uani 1 1 d . . . H11A H 0.4880 0.3108 0.5141 0.041 Uiso 1 1 calc R . . H11B H 0.4861 0.1975 0.5524 0.041 Uiso 1 1 calc R . . H11C H 0.4066 0.2940 0.5634 0.041 Uiso 1 1 calc R . . C12 C 0.09636(12) 0.09078(13) 0.37570(7) 0.0160(3) Uani 1 1 d . . . C13 C 0.07318(12) -0.01589(14) 0.35206(7) 0.0174(3) Uani 1 1 d . . . C14 C -0.02459(13) -0.03436(15) 0.32479(8) 0.0219(4) Uani 1 1 d . . . H14 H -0.0422 -0.1058 0.3087 0.026 Uiso 1 1 calc R . . C15 C -0.09628(13) 0.04978(16) 0.32087(8) 0.0250(4) Uani 1 1 d . . . H15 H -0.1620 0.0361 0.3016 0.030 Uiso 1 1 calc R . . C16 C -0.07224(13) 0.15327(15) 0.34495(8) 0.0224(4) Uani 1 1 d . . . H16 H -0.1220 0.2102 0.3423 0.027 Uiso 1 1 calc R . . C17 C 0.02387(12) 0.17589(14) 0.37316(8) 0.0182(3) Uani 1 1 d . . . C18 C 0.14677(13) -0.11366(14) 0.35649(8) 0.0197(4) Uani 1 1 d . . . H18 H 0.2162 -0.0842 0.3681 0.024 Uiso 1 1 calc R . . C19 C 0.14854(14) -0.17551(15) 0.29510(9) 0.0258(4) Uani 1 1 d . . . H19A H 0.0835 -0.2129 0.2854 0.039 Uiso 1 1 calc R . . H19B H 0.2030 -0.2308 0.2982 0.039 Uiso 1 1 calc R . . H19C H 0.1602 -0.1223 0.2625 0.039 Uiso 1 1 calc R . . C20 C 0.11993(15) -0.19659(15) 0.40619(9) 0.0283(4) Uani 1 1 d . . . H20A H 0.1237 -0.1592 0.4462 0.042 Uiso 1 1 calc R . . H20B H 0.1678 -0.2588 0.4078 0.042 Uiso 1 1 calc R . . H20C H 0.0512 -0.2246 0.3963 0.042 Uiso 1 1 calc R . . C21 C 0.04562(13) 0.29177(14) 0.39910(8) 0.0218(4) Uani 1 1 d . . . H21 H 0.1155 0.2916 0.4201 0.026 Uiso 1 1 calc R . . C22 C 0.04219(15) 0.37828(16) 0.34796(9) 0.0305(4) Uani 1 1 d . . . H22A H 0.0898 0.3574 0.3179 0.046 Uiso 1 1 calc R . . H22B H 0.0610 0.4511 0.3655 0.046 Uiso 1 1 calc R . . H22C H -0.0264 0.3820 0.3276 0.046 Uiso 1 1 calc R . . C23 C -0.02798(17) 0.32366(17) 0.44661(10) 0.0351(5) Uani 1 1 d . . . H23A H -0.0966 0.3292 0.4264 0.053 Uiso 1 1 calc R . . H23B H -0.0080 0.3955 0.4650 0.053 Uiso 1 1 calc R . . H23C H -0.0264 0.2667 0.4788 0.053 Uiso 1 1 calc R . . C24 C 0.44977(12) 0.31071(13) 0.40653(7) 0.0159(3) Uani 1 1 d . . . C25 C 0.55145(12) 0.27971(14) 0.40275(8) 0.0193(3) Uani 1 1 d . . . C26 C 0.61858(13) 0.36035(15) 0.38429(8) 0.0237(4) Uani 1 1 d . . . H26 H 0.6874 0.3407 0.3814 0.028 Uiso 1 1 calc R . . C27 C 0.58785(14) 0.46740(15) 0.37019(8) 0.0246(4) Uani 1 1 d . . . H27 H 0.6348 0.5207 0.3576 0.030 Uiso 1 1 calc R . . C28 C 0.48772(14) 0.49623(14) 0.37456(8) 0.0231(4) Uani 1 1 d . . . H28 H 0.4667 0.5702 0.3652 0.028 Uiso 1 1 calc R . . C29 C 0.41666(13) 0.41935(14) 0.39234(8) 0.0187(3) Uani 1 1 d . . . C30 C 0.59285(13) 0.16425(15) 0.41818(9) 0.0263(4) Uani 1 1 d . . . H30 H 0.5370 0.1177 0.4325 0.032 Uiso 1 1 calc R . . C31 C 0.63050(15) 0.10978(17) 0.36067(11) 0.0371(5) Uani 1 1 d . . . H31A H 0.5757 0.1088 0.3277 0.056 Uiso 1 1 calc R . . H31B H 0.6521 0.0334 0.3703 0.056 Uiso 1 1 calc R . . H31C H 0.6877 0.1523 0.3473 0.056 Uiso 1 1 calc R . . C32 C 0.67911(15) 0.16914(18) 0.46981(11) 0.0393(5) Uani 1 1 d . . . H32A H 0.7374 0.2076 0.4549 0.059 Uiso 1 1 calc R . . H32B H 0.6988 0.0935 0.4823 0.059 Uiso 1 1 calc R . . H32C H 0.6561 0.2094 0.5051 0.059 Uiso 1 1 calc R . . C33 C 0.30848(13) 0.45779(14) 0.39769(9) 0.0243(4) Uani 1 1 d . . . H33 H 0.2646 0.3902 0.3978 0.029 Uiso 1 1 calc R . . C34 C 0.26997(17) 0.5296(2) 0.34295(13) 0.0530(7) Uani 1 1 d . . . H34A H 0.3092 0.5986 0.3431 0.080 Uiso 1 1 calc R . . H34B H 0.1984 0.5473 0.3459 0.080 Uiso 1 1 calc R . . H34C H 0.2775 0.4890 0.3047 0.080 Uiso 1 1 calc R . . C35 C 0.29995(19) 0.5188(3) 0.45795(13) 0.0624(8) Uani 1 1 d . . . H35A H 0.3245 0.4709 0.4923 0.094 Uiso 1 1 calc R . . H35B H 0.2291 0.5383 0.4619 0.094 Uiso 1 1 calc R . . H35C H 0.3408 0.5868 0.4585 0.094 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 C1 0.0161(8) 0.0192(8) 0.0195(8) -0.0002(6) 0.0034(6) 0.0001(6) N1 0.0182(7) 0.0227(7) 0.0197(7) -0.0018(6) 0.0023(6) 0.0041(6) O1 0.0168(6) 0.0189(6) 0.0187(6) -0.0021(5) -0.0010(5) 0.0022(5) Si1 0.0127(2) 0.0160(2) 0.0149(2) 0.00079(17) 0.00133(16) -0.00018(17) C2 0.0394(12) 0.0327(11) 0.0265(10) -0.0101(8) -0.0011(8) 0.0141(9) N2 0.0159(7) 0.0207(7) 0.0155(7) -0.0003(5) 0.0011(5) 0.0025(5) O2 0.0227(6) 0.0219(6) 0.0240(7) -0.0039(5) -0.0019(5) 0.0080(5) C3 0.0386(12) 0.0329(10) 0.0293(11) -0.0005(8) 0.0111(9) 0.0140(9) N3 0.0121(6) 0.0175(7) 0.0149(7) 0.0004(5) 0.0003(5) -0.0023(5) O3 0.0215(7) 0.0321(7) 0.0254(7) 0.0039(5) 0.0015(5) 0.0089(5) C4 0.0160(8) 0.0328(10) 0.0177(9) 0.0018(7) 0.0025(7) 0.0020(7) N4 0.0124(6) 0.0142(6) 0.0171(7) 0.0009(5) 0.0015(5) -0.0003(5) O4 0.0220(15) 0.024(2) 0.0114(13) 0.0031(13) -0.0015(10) 0.0036(16) C5 0.0212(18) 0.022(2) 0.0159(16) 0.0072(17) -0.0030(12) -0.0007(17) C6 0.0267(16) 0.0340(17) 0.0265(17) 0.0123(14) 0.0017(13) -0.0006(13) O4' 0.024(4) 0.034(5) 0.018(3) 0.007(3) 0.003(2) 0.015(4) C5' 0.028(4) 0.031(5) 0.021(3) 0.010(4) -0.006(3) 0.004(4) C6' 0.036(3) 0.043(4) 0.024(3) 0.001(2) -0.005(2) 0.003(3) C7 0.0214(9) 0.0295(9) 0.0193(9) 0.0025(7) 0.0046(7) -0.0071(7) C8 0.0180(8) 0.0184(8) 0.0175(8) 0.0027(6) 0.0025(6) -0.0007(6) C9 0.0214(9) 0.0253(9) 0.0144(8) 0.0046(7) -0.0003(6) -0.0047(7) C10 0.0165(8) 0.0194(8) 0.0182(8) 0.0001(6) -0.0008(6) -0.0003(6) C11 0.0248(10) 0.0386(11) 0.0187(9) -0.0005(8) -0.0015(7) -0.0114(8) C12 0.0116(8) 0.0211(8) 0.0153(8) 0.0020(6) 0.0007(6) -0.0024(6) C13 0.0158(8) 0.0207(8) 0.0157(8) 0.0007(6) 0.0020(6) -0.0017(6) C14 0.0181(9) 0.0242(9) 0.0230(9) -0.0038(7) -0.0005(7) -0.0046(7) C15 0.0122(8) 0.0342(10) 0.0278(10) -0.0038(8) -0.0023(7) -0.0020(7) C16 0.0137(8) 0.0273(9) 0.0258(9) 0.0006(7) 0.0006(7) 0.0034(7) C17 0.0143(8) 0.0212(8) 0.0194(8) 0.0006(6) 0.0037(6) -0.0012(6) C18 0.0183(8) 0.0175(8) 0.0229(9) -0.0009(7) -0.0016(7) -0.0014(6) C19 0.0263(10) 0.0223(9) 0.0287(10) -0.0036(7) 0.0018(8) 0.0010(7) C20 0.0299(10) 0.0234(9) 0.0310(10) 0.0035(8) -0.0009(8) -0.0020(8) C21 0.0171(8) 0.0207(8) 0.0274(9) -0.0014(7) 0.0000(7) 0.0023(7) C22 0.0350(11) 0.0233(9) 0.0332(11) 0.0013(8) 0.0031(8) 0.0012(8) C23 0.0434(12) 0.0274(10) 0.0363(12) -0.0076(9) 0.0129(9) 0.0006(9) C24 0.0153(8) 0.0178(8) 0.0144(8) -0.0010(6) 0.0008(6) -0.0040(6) C25 0.0167(8) 0.0210(8) 0.0200(8) -0.0025(7) 0.0003(6) -0.0019(6) C26 0.0153(8) 0.0320(10) 0.0243(9) -0.0055(7) 0.0046(7) -0.0056(7) C27 0.0265(10) 0.0274(9) 0.0203(9) -0.0003(7) 0.0043(7) -0.0118(7) C28 0.0269(9) 0.0187(8) 0.0231(9) 0.0009(7) -0.0004(7) -0.0052(7) C29 0.0202(9) 0.0176(8) 0.0182(8) -0.0019(6) 0.0003(7) -0.0022(6) C30 0.0141(8) 0.0228(9) 0.0412(11) -0.0013(8) -0.0016(7) 0.0006(7) C31 0.0227(10) 0.0297(11) 0.0603(15) -0.0119(10) 0.0114(9) 0.0011(8) C32 0.0228(10) 0.0307(11) 0.0614(15) 0.0031(10) -0.0136(10) 0.0011(8) C33 0.0204(9) 0.0157(8) 0.0364(11) -0.0008(7) 0.0006(7) 0.0002(7) C34 0.0299(12) 0.0479(14) 0.0804(19) 0.0342(13) -0.0008(12) 0.0058(10) C35 0.0333(13) 0.085(2) 0.0696(18) -0.0419(16) 0.0059(12) 0.0142(13) _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 C1 N1 1.272(2) . ? C1 O1 1.340(2) . ? C1 O2 1.342(2) . ? N1 N2 1.4275(19) . ? O1 Si1 1.7205(12) . ? Si1 N3 1.8078(14) . ? Si1 N2 1.8405(14) . ? Si1 N4 1.9272(14) . ? Si1 H1S 1.371(19) . ? C2 O2 1.452(2) . ? C2 C3 1.491(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C4 1.353(2) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? N3 C8 1.364(2) . ? N3 C12 1.467(2) . ? O3 C4 1.221(2) . ? C4 O4' 1.330(10) . ? C4 O4 1.388(5) . ? N4 C10 1.315(2) . ? N4 C24 1.457(2) . ? O4 C5 1.451(6) . ? C5 C6 1.509(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O4' C5' 1.449(10) . ? C5' C6' 1.478(10) . ? C5' H5'1 0.9900 . ? C5' H5'2 0.9900 . ? C6' H6'1 0.9800 . ? C6' H6'2 0.9800 . ? C6' H6'3 0.9800 . ? C7 C8 1.510(2) . ? C7 H7S1 0.9800 . ? C7 H7S2 0.9800 . ? C7 H7S3 0.9800 . ? C8 C9 1.375(2) . ? C9 C10 1.408(2) . ? C9 H9 0.9500 . ? C10 C11 1.505(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C17 1.403(2) . ? C12 C13 1.408(2) . ? C13 C14 1.399(2) . ? C13 C18 1.527(2) . ? C14 C15 1.387(3) . ? C14 H14 0.9500 . ? C15 C16 1.379(3) . ? C15 H15 0.9500 . ? C16 C17 1.396(2) . ? C16 H16 0.9500 . ? C17 C21 1.524(2) . ? C18 C19 1.535(2) . ? C18 C20 1.538(2) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.525(3) . ? C21 C23 1.532(3) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C29 1.406(2) . ? C24 C25 1.409(2) . ? C25 C26 1.399(2) . ? C25 C30 1.521(2) . ? C26 C27 1.378(3) . ? C26 H26 0.9500 . ? C27 C28 1.384(3) . ? C27 H27 0.9500 . ? C28 C29 1.399(2) . ? C28 H28 0.9500 . ? C29 C33 1.522(2) . ? C30 C31 1.537(3) . ? C30 C32 1.539(3) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.520(3) . ? C33 C34 1.528(3) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 O1 122.46(15) . . ? N1 C1 O2 125.49(15) . . ? O1 C1 O2 112.05(14) . . ? C1 N1 N2 105.16(13) . . ? C1 O1 Si1 113.76(10) . . ? O1 Si1 N3 108.85(6) . . ? O1 Si1 N2 83.74(6) . . ? N3 Si1 N2 100.83(6) . . ? O1 Si1 N4 85.23(6) . . ? N3 Si1 N4 94.72(6) . . ? N2 Si1 N4 163.19(6) . . ? O1 Si1 H1S 135.7(8) . . ? N3 Si1 H1S 115.4(8) . . ? N2 Si1 H1S 90.7(8) . . ? N4 Si1 H1S 88.4(8) . . ? O2 C2 C3 108.04(16) . . ? O2 C2 H2A 110.1 . . ? C3 C2 H2A 110.1 . . ? O2 C2 H2B 110.1 . . ? C3 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C4 N2 N1 118.62(14) . . ? C4 N2 Si1 124.10(12) . . ? N1 N2 Si1 114.81(10) . . ? C1 O2 C2 115.19(13) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C8 N3 C12 116.63(13) . . ? C8 N3 Si1 123.61(11) . . ? C12 N3 Si1 119.76(10) . . ? O3 C4 O4' 117.1(5) . . ? O3 C4 N2 122.82(16) . . ? O4' C4 N2 118.9(5) . . ? O3 C4 O4 125.6(3) . . ? N2 C4 O4 111.2(3) . . ? C10 N4 C24 119.52(13) . . ? C10 N4 Si1 124.44(11) . . ? C24 N4 Si1 115.83(10) . . ? C4 O4 C5 112.9(4) . . ? O4 C5 C6 111.2(3) . . ? O4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? O4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 O4' C5' 116.4(8) . . ? O4' C5' C6' 106.8(7) . . ? O4' C5' H5'1 110.4 . . ? C6' C5' H5'1 110.4 . . ? O4' C5' H5'2 110.4 . . ? C6' C5' H5'2 110.4 . . ? H5'1 C5' H5'2 108.6 . . ? C5' C6' H6'1 109.5 . . ? C5' C6' H6'2 109.5 . . ? H6'1 C6' H6'2 109.5 . . ? C5' C6' H6'3 109.5 . . ? H6'1 C6' H6'3 109.5 . . ? H6'2 C6' H6'3 109.5 . . ? C8 C7 H7S1 109.5 . . ? C8 C7 H7S2 109.5 . . ? H7S1 C7 H7S2 109.5 . . ? C8 C7 H7S3 109.5 . . ? H7S1 C7 H7S3 109.5 . . ? H7S2 C7 H7S3 109.5 . . ? N3 C8 C9 123.90(15) . . ? N3 C8 C7 118.81(14) . . ? C9 C8 C7 117.21(15) . . ? C8 C9 C10 125.98(16) . . ? C8 C9 H9 117.0 . . ? C10 C9 H9 117.0 . . ? N4 C10 C9 120.70(15) . . ? N4 C10 C11 122.19(15) . . ? C9 C10 C11 117.03(15) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 121.54(15) . . ? C17 C12 N3 118.16(14) . . ? C13 C12 N3 120.29(14) . . ? C14 C13 C12 117.86(15) . . ? C14 C13 C18 118.02(15) . . ? C12 C13 C18 124.08(14) . . ? C15 C14 C13 121.13(16) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 C14 120.01(16) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 121.21(16) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C12 118.23(15) . . ? C16 C17 C21 118.70(15) . . ? C12 C17 C21 123.06(15) . . ? C13 C18 C19 112.00(14) . . ? C13 C18 C20 111.12(14) . . ? C19 C18 C20 108.84(14) . . ? C13 C18 H18 108.3 . . ? C19 C18 H18 108.3 . . ? C20 C18 H18 108.3 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C21 C22 111.07(15) . . ? C17 C21 C23 111.68(15) . . ? C22 C21 C23 110.07(15) . . ? C17 C21 H21 108.0 . . ? C22 C21 H21 108.0 . . ? C23 C21 H21 108.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29 C24 C25 121.10(15) . . ? C29 C24 N4 118.20(14) . . ? C25 C24 N4 120.69(14) . . ? C26 C25 C24 117.97(16) . . ? C26 C25 C30 118.07(15) . . ? C24 C25 C30 123.96(15) . . ? C27 C26 C25 121.95(16) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C28 119.13(16) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? C27 C28 C29 121.76(17) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C28 C29 C24 118.09(15) . . ? C28 C29 C33 118.82(15) . . ? C24 C29 C33 123.04(15) . . ? C25 C30 C31 110.15(16) . . ? C25 C30 C32 111.10(15) . . ? C31 C30 C32 110.03(16) . . ? C25 C30 H30 108.5 . . ? C31 C30 H30 108.5 . . ? C32 C30 H30 108.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C35 C33 C29 110.62(16) . . ? C35 C33 C34 111.1(2) . . ? C29 C33 C34 111.59(16) . . ? C35 C33 H33 107.8 . . ? C29 C33 H33 107.8 . . ? C34 C33 H33 107.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 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 O1 C1 N1 N2 -2.7(2) . . . . ? O2 C1 N1 N2 177.90(15) . . . . ? N1 C1 O1 Si1 1.5(2) . . . . ? O2 C1 O1 Si1 -179.10(10) . . . . ? C1 O1 Si1 N3 99.70(11) . . . . ? C1 O1 Si1 N2 0.36(11) . . . . ? C1 O1 Si1 N4 -166.93(11) . . . . ? C1 N1 N2 C4 165.70(15) . . . . ? C1 N1 N2 Si1 2.81(16) . . . . ? O1 Si1 N2 C4 -163.67(14) . . . . ? N3 Si1 N2 C4 88.28(14) . . . . ? N4 Si1 N2 C4 -114.4(2) . . . . ? O1 Si1 N2 N1 -1.84(11) . . . . ? N3 Si1 N2 N1 -109.90(11) . . . . ? N4 Si1 N2 N1 47.5(3) . . . . ? N1 C1 O2 C2 1.6(2) . . . . ? O1 C1 O2 C2 -177.86(15) . . . . ? C3 C2 O2 C1 168.01(16) . . . . ? O1 Si1 N3 C8 63.25(14) . . . . ? N2 Si1 N3 C8 150.27(13) . . . . ? N4 Si1 N3 C8 -23.31(14) . . . . ? O1 Si1 N3 C12 -116.83(12) . . . . ? N2 Si1 N3 C12 -29.81(13) . . . . ? N4 Si1 N3 C12 156.61(12) . . . . ? N1 N2 C4 O3 -178.25(15) . . . . ? Si1 N2 C4 O3 -17.1(2) . . . . ? N1 N2 C4 O4' -11.1(5) . . . . ? Si1 N2 C4 O4' 150.0(5) . . . . ? N1 N2 C4 O4 7.8(3) . . . . ? Si1 N2 C4 O4 169.0(2) . . . . ? O1 Si1 N4 C10 -83.23(14) . . . . ? N3 Si1 N4 C10 25.34(14) . . . . ? N2 Si1 N4 C10 -132.4(2) . . . . ? O1 Si1 N4 C24 91.44(11) . . . . ? N3 Si1 N4 C24 -159.99(11) . . . . ? N2 Si1 N4 C24 42.3(3) . . . . ? O3 C4 O4 C5 5.5(5) . . . . ? O4' C4 O4 C5 -63(2) . . . . ? N2 C4 O4 C5 179.2(3) . . . . ? C4 O4 C5 C6 80.6(5) . . . . ? O3 C4 O4' C5' -8.6(9) . . . . ? N2 C4 O4' C5' -176.4(5) . . . . ? O4 C4 O4' C5' 113(3) . . . . ? C4 O4' C5' C6' -178.8(7) . . . . ? C12 N3 C8 C9 -170.10(16) . . . . ? Si1 N3 C8 C9 9.8(2) . . . . ? C12 N3 C8 C7 6.6(2) . . . . ? Si1 N3 C8 C7 -173.52(12) . . . . ? N3 C8 C9 C10 12.4(3) . . . . ? C7 C8 C9 C10 -164.30(17) . . . . ? C24 N4 C10 C9 173.16(15) . . . . ? Si1 N4 C10 C9 -12.4(2) . . . . ? C24 N4 C10 C11 -3.5(2) . . . . ? Si1 N4 C10 C11 171.01(13) . . . . ? C8 C9 C10 N4 -10.4(3) . . . . ? C8 C9 C10 C11 166.41(17) . . . . ? C8 N3 C12 C17 83.83(18) . . . . ? Si1 N3 C12 C17 -96.09(15) . . . . ? C8 N3 C12 C13 -94.69(18) . . . . ? Si1 N3 C12 C13 85.38(17) . . . . ? C17 C12 C13 C14 1.0(2) . . . . ? N3 C12 C13 C14 179.50(14) . . . . ? C17 C12 C13 C18 -176.56(15) . . . . ? N3 C12 C13 C18 1.9(2) . . . . ? C12 C13 C14 C15 0.3(3) . . . . ? C18 C13 C14 C15 178.06(16) . . . . ? C13 C14 C15 C16 -1.0(3) . . . . ? C14 C15 C16 C17 0.4(3) . . . . ? C15 C16 C17 C12 0.9(3) . . . . ? C15 C16 C17 C21 -179.76(16) . . . . ? C13 C12 C17 C16 -1.6(2) . . . . ? N3 C12 C17 C16 179.88(14) . . . . ? C13 C12 C17 C21 179.05(15) . . . . ? N3 C12 C17 C21 0.5(2) . . . . ? C14 C13 C18 C19 48.4(2) . . . . ? C12 C13 C18 C19 -134.01(17) . . . . ? C14 C13 C18 C20 -73.56(19) . . . . ? C12 C13 C18 C20 104.03(18) . . . . ? C16 C17 C21 C22 -66.0(2) . . . . ? C12 C17 C21 C22 113.35(18) . . . . ? C16 C17 C21 C23 57.3(2) . . . . ? C12 C17 C21 C23 -123.35(18) . . . . ? C10 N4 C24 C29 -100.41(18) . . . . ? Si1 N4 C24 C29 84.65(16) . . . . ? C10 N4 C24 C25 80.0(2) . . . . ? Si1 N4 C24 C25 -94.93(16) . . . . ? C29 C24 C25 C26 -0.1(2) . . . . ? N4 C24 C25 C26 179.44(15) . . . . ? C29 C24 C25 C30 179.18(16) . . . . ? N4 C24 C25 C30 -1.3(2) . . . . ? C24 C25 C26 C27 0.2(3) . . . . ? C30 C25 C26 C27 -179.17(17) . . . . ? C25 C26 C27 C28 0.2(3) . . . . ? C26 C27 C28 C29 -0.6(3) . . . . ? C27 C28 C29 C24 0.6(3) . . . . ? C27 C28 C29 C33 178.47(16) . . . . ? C25 C24 C29 C28 -0.3(2) . . . . ? N4 C24 C29 C28 -179.85(14) . . . . ? C25 C24 C29 C33 -178.00(16) . . . . ? N4 C24 C29 C33 2.4(2) . . . . ? C26 C25 C30 C31 -64.3(2) . . . . ? C24 C25 C30 C31 116.44(18) . . . . ? C26 C25 C30 C32 57.9(2) . . . . ? C24 C25 C30 C32 -121.38(19) . . . . ? C28 C29 C33 C35 -79.6(2) . . . . ? C24 C29 C33 C35 98.1(2) . . . . ? C28 C29 C33 C34 44.6(2) . . . . ? C24 C29 C33 C34 -137.64(19) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 21.07 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.337 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.048 data_817514 _database_code_depnum_ccdc_archive 'CCDC 817515' #TrackingRef 'azhakar_tolylhydra.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H48 N4 O Si, 0.52(C6 H14)' _chemical_formula_sum 'C39.12 H55.24 N4 O Si' _chemical_formula_weight 625.654 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.4828(8) _cell_length_b 12.0258(9) _cell_length_c 26.1609(19) _cell_angle_alpha 90.00 _cell_angle_beta 94.746(2) _cell_angle_gamma 90.00 _cell_volume 3600.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9029 _cell_measurement_theta_min 2.304 _cell_measurement_theta_max 25.499 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.933 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details 'SADABS 2008/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Mo rotating anode' _diffrn_radiation_monochromator 'mirror optics' _diffrn_measurement_device_type 'Bruker APEX II Ultra' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 57531 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.11 _reflns_number_total 7146 _reflns_number_gt 6108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2008.11' _computing_cell_refinement 'SAINT V7.68A' _computing_data_reduction 'SAINT V7.46A' _computing_structure_solution 'SHELXS in SHELXTL Version 2008/3' _computing_structure_refinement 'SHELXL in SHELXTL Version 2008/3' _computing_molecular_graphics 'XSHELL in SHELXTL-97' _computing_publication_material 'XSHELL in SHELXTL-97' _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^)+(0.0407P)^2^+1.8475P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7146 _refine_ls_number_parameters 434 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.98897(3) 0.16926(3) 0.164499(13) 0.01451(9) Uani 1 1 d . . . H1S H 0.9928(13) 0.2757(12) 0.1838(6) 0.017(4) Uiso 1 1 d . . . O1 O 1.13074(8) 0.13396(8) 0.19090(3) 0.0172(2) Uani 1 1 d . . . N1 N 0.83727(10) 0.19651(9) 0.12801(4) 0.0164(2) Uani 1 1 d . . . N2 N 0.92315(9) 0.08556(9) 0.21331(4) 0.0147(2) Uani 1 1 d . . . N3 N 1.04136(10) 0.12553(10) 0.10733(4) 0.0186(2) Uani 1 1 d . . . H3N H 0.9986 0.1317 0.0780 0.022 Uiso 1 1 calc R . . N4 N 1.15409(10) 0.08003(10) 0.10960(4) 0.0195(3) Uani 1 1 d . . . C1 C 0.74172(12) 0.21066(11) 0.15237(5) 0.0181(3) Uani 1 1 d . . . C2 C 0.73522(12) 0.17480(12) 0.20299(5) 0.0182(3) Uani 1 1 d D . . H2 H 0.6631(14) 0.1871(13) 0.2169(6) 0.022 Uiso 1 1 d D . . C3 C 0.81619(12) 0.10584(11) 0.22922(5) 0.0156(3) Uani 1 1 d . . . C4 C 0.63258(12) 0.26138(14) 0.12587(6) 0.0251(3) Uani 1 1 d . . . H4A H 0.6451 0.2765 0.0899 0.038 Uiso 0.260(18) 1 calc PR . . H4B H 0.6147 0.3311 0.1430 0.038 Uiso 0.260(18) 1 calc PR . . H4C H 0.5671 0.2095 0.1275 0.038 Uiso 0.260(18) 1 calc PR . . H4D H 0.5728 0.2682 0.1503 0.038 Uiso 0.740(18) 1 calc PR . . H4E H 0.6033 0.2136 0.0973 0.038 Uiso 0.740(18) 1 calc PR . . H4F H 0.6508 0.3352 0.1128 0.038 Uiso 0.740(18) 1 calc PR . . C5 C 0.77952(12) 0.04896(12) 0.27673(5) 0.0197(3) Uani 1 1 d . . . H5A H 0.7932 -0.0312 0.2742 0.030 Uiso 1 1 calc R . . H5B H 0.6963 0.0626 0.2798 0.030 Uiso 1 1 calc R . . H5C H 0.8253 0.0786 0.3070 0.030 Uiso 1 1 calc R . . C6 C 0.82988(12) 0.22508(12) 0.07386(5) 0.0194(3) Uani 1 1 d . . . C7 C 0.80070(12) 0.14208(13) 0.03721(5) 0.0220(3) Uani 1 1 d . . . C8 C 0.79842(13) 0.17081(14) -0.01463(6) 0.0282(3) Uani 1 1 d . . . H8 H 0.7809 0.1156 -0.0401 0.034 Uiso 1 1 calc R . . C9 C 0.82130(15) 0.27833(15) -0.02932(6) 0.0326(4) Uani 1 1 d . . . H9 H 0.8186 0.2968 -0.0647 0.039 Uiso 1 1 calc R . . C10 C 0.84800(14) 0.35882(14) 0.00722(6) 0.0299(4) Uani 1 1 d . . . H10 H 0.8627 0.4327 -0.0034 0.036 Uiso 1 1 calc R . . C11 C 0.85398(13) 0.33450(13) 0.05951(5) 0.0238(3) Uani 1 1 d . . . C12 C 0.77024(13) 0.02362(13) 0.05184(5) 0.0247(3) Uani 1 1 d . . . H12 H 0.7788 0.0178 0.0901 0.030 Uiso 1 1 calc R . . C13 C 0.64300(14) -0.00297(16) 0.03350(6) 0.0362(4) Uani 1 1 d . . . H13A H 0.5912 0.0513 0.0480 0.054 Uiso 1 1 calc R . . H13B H 0.6235 -0.0779 0.0448 0.054 Uiso 1 1 calc R . . H13C H 0.6330 0.0007 -0.0040 0.054 Uiso 1 1 calc R . . C14 C 0.85179(14) -0.06235(13) 0.03009(6) 0.0296(3) Uani 1 1 d . . . H14A H 0.8441 -0.0586 -0.0075 0.044 Uiso 1 1 calc R . . H14B H 0.8306 -0.1370 0.0411 0.044 Uiso 1 1 calc R . . H14C H 0.9328 -0.0463 0.0427 0.044 Uiso 1 1 calc R . . C15 C 0.88702(14) 0.42577(13) 0.09836(6) 0.0277(3) Uani 1 1 d . . . H15 H 0.8722 0.3970 0.1331 0.033 Uiso 1 1 calc R . . C16 C 0.81220(18) 0.53048(14) 0.08821(7) 0.0396(4) Uani 1 1 d . . . H16A H 0.8295 0.5636 0.0554 0.059 Uiso 1 1 calc R . . H16B H 0.8301 0.5842 0.1159 0.059 Uiso 1 1 calc R . . H16C H 0.7293 0.5105 0.0868 0.059 Uiso 1 1 calc R . . C17 C 1.01738(16) 0.45313(15) 0.09892(7) 0.0390(4) Uani 1 1 d . . . H17A H 1.0344 0.4812 0.0652 0.058 Uiso 1 1 calc R . . H17B H 1.0634 0.3858 0.1069 0.058 Uiso 1 1 calc R . . H17C H 1.0378 0.5099 0.1250 0.058 Uiso 1 1 calc R . . C18 C 0.99576(11) 0.00604(11) 0.24352(5) 0.0152(3) Uani 1 1 d . . . C19 C 1.00765(11) -0.10101(11) 0.22328(5) 0.0170(3) Uani 1 1 d . . . C20 C 1.07268(12) -0.17885(12) 0.25329(5) 0.0204(3) Uani 1 1 d . . . H20 H 1.0809 -0.2523 0.2407 0.025 Uiso 1 1 calc R . . C21 C 1.12525(12) -0.15086(12) 0.30109(5) 0.0214(3) Uani 1 1 d . . . H21 H 1.1683 -0.2051 0.3212 0.026 Uiso 1 1 calc R . . C22 C 1.11503(12) -0.04371(12) 0.31957(5) 0.0201(3) Uani 1 1 d . . . H22 H 1.1523 -0.0250 0.3522 0.024 Uiso 1 1 calc R . . C23 C 1.05108(11) 0.03735(11) 0.29123(5) 0.0166(3) Uani 1 1 d . . . C24 C 0.95212(12) -0.13082(11) 0.17011(5) 0.0187(3) Uani 1 1 d . . . H24 H 0.9548 -0.0624 0.1485 0.022 Uiso 1 1 calc R . . C25 C 0.82339(13) -0.16276(13) 0.17133(6) 0.0268(3) Uani 1 1 d . . . H25A H 0.8167 -0.2260 0.1945 0.040 Uiso 1 1 calc R . . H25B H 0.7914 -0.1833 0.1367 0.040 Uiso 1 1 calc R . . H25C H 0.7797 -0.0994 0.1835 0.040 Uiso 1 1 calc R . . C26 C 1.01907(15) -0.22095(15) 0.14409(7) 0.0378(4) Uani 1 1 d . . . H26A H 1.1013 -0.1992 0.1440 0.057 Uiso 1 1 calc R . . H26B H 0.9855 -0.2307 0.1087 0.057 Uiso 1 1 calc R . . H26C H 1.0136 -0.2911 0.1628 0.057 Uiso 1 1 calc R . . C27 C 1.04959(12) 0.15590(11) 0.31199(5) 0.0178(3) Uani 1 1 d . . . H27 H 0.9918 0.1999 0.2896 0.021 Uiso 1 1 calc R . . C28 C 1.01413(13) 0.16162(13) 0.36730(5) 0.0244(3) Uani 1 1 d . . . H28A H 0.9403 0.1218 0.3696 0.037 Uiso 1 1 calc R . . H28B H 1.0044 0.2395 0.3771 0.037 Uiso 1 1 calc R . . H28C H 1.0751 0.1271 0.3905 0.037 Uiso 1 1 calc R . . C29 C 1.16996(12) 0.21050(12) 0.31029(5) 0.0213(3) Uani 1 1 d . . . H29A H 1.2289 0.1658 0.3302 0.032 Uiso 1 1 calc R . . H29B H 1.1681 0.2854 0.3249 0.032 Uiso 1 1 calc R . . H29C H 1.1898 0.2152 0.2746 0.032 Uiso 1 1 calc R . . C31 C 1.19619(12) 0.08731(11) 0.15664(5) 0.0164(3) Uani 1 1 d . . . C32 C 1.31109(12) 0.04220(11) 0.17490(5) 0.0176(3) Uani 1 1 d . . . C33 C 1.39575(12) 0.01944(12) 0.14090(6) 0.0219(3) Uani 1 1 d . . . H33 H 1.3808 0.0364 0.1055 0.026 Uiso 1 1 calc R . . C34 C 1.50142(12) -0.02785(13) 0.15878(6) 0.0248(3) Uani 1 1 d . . . H34 H 1.5590 -0.0426 0.1356 0.030 Uiso 1 1 calc R . . C35 C 1.52363(12) -0.05374(12) 0.21038(6) 0.0241(3) Uani 1 1 d . . . H35 H 1.5954 -0.0878 0.2223 0.029 Uiso 1 1 calc R . . C36 C 1.44080(13) -0.02977(12) 0.24435(6) 0.0230(3) Uani 1 1 d . . . H36 H 1.4563 -0.0464 0.2798 0.028 Uiso 1 1 calc R . . C37 C 1.33509(12) 0.01851(11) 0.22680(5) 0.0197(3) Uani 1 1 d . . . H37 H 1.2789 0.0355 0.2503 0.024 Uiso 1 1 calc R . . C38 C 0.46090(15) 0.47169(14) 0.01824(6) 0.0317(4) Uani 0.761(6) 1 d P . 1 H38A H 0.4984 0.4778 0.0536 0.038 Uiso 0.761(6) 1 calc PR . 1 H38B H 0.3858 0.5123 0.0171 0.038 Uiso 0.761(6) 1 calc PR . 1 C39 C 0.43561(16) 0.34981(14) 0.00667(6) 0.0338(4) Uani 0.761(6) 1 d P . 1 H39A H 0.5104 0.3085 0.0081 0.041 Uiso 0.761(6) 1 calc PR . 1 H39B H 0.3981 0.3432 -0.0286 0.041 Uiso 0.761(6) 1 calc PR . 1 C40 C 0.35677(19) 0.29663(16) 0.04374(7) 0.0351(5) Uani 0.761(6) 1 d P . 1 H40A H 0.3437 0.2184 0.0345 0.053 Uiso 0.761(6) 1 calc PR . 1 H40B H 0.2817 0.3358 0.0419 0.053 Uiso 0.761(6) 1 calc PR . 1 H40C H 0.3941 0.3014 0.0787 0.053 Uiso 0.761(6) 1 calc PR . 1 C37' C 0.46090(15) 0.47169(14) 0.01824(6) 0.0317(4) Uani 0.239(6) 1 d P . 2 H37A H 0.4984 0.4778 0.0536 0.038 Uiso 0.239(6) 1 calc PR . 2 H37B H 0.3858 0.5123 0.0171 0.038 Uiso 0.239(6) 1 calc PR . 2 C38' C 0.43561(16) 0.34981(14) 0.00667(6) 0.0338(4) Uani 0.239(6) 1 d P . 2 H38C H 0.5104 0.3085 0.0081 0.041 Uiso 0.239(6) 1 calc PR . 2 H38D H 0.3981 0.3432 -0.0286 0.041 Uiso 0.239(6) 1 calc PR . 2 C39' C 0.35677(19) 0.29663(16) 0.04374(7) 0.0351(5) Uani 0.120(3) 1 d PD . 2 H39C H 0.3554 0.2159 0.0363 0.042 Uiso 0.120(3) 1 calc PR . 2 H39D H 0.3965 0.3056 0.0785 0.042 Uiso 0.120(3) 1 calc PR . 2 C40' C 0.2500(5) 0.3267(5) 0.0465(2) 0.0245(19) Uani 0.239(6) 1 d PD . 2 H40D H 0.2151 0.2825 0.0727 0.037 Uiso 0.239(6) 1 calc PR . 2 H40E H 0.2060 0.3149 0.0132 0.037 Uiso 0.239(6) 1 calc PR . 2 H40F H 0.2475 0.4057 0.0556 0.037 Uiso 0.239(6) 1 calc PR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.01556(18) 0.01521(18) 0.01280(17) 0.00027(14) 0.00140(13) -0.00033(14) O1 0.0157(5) 0.0214(5) 0.0144(4) -0.0008(4) 0.0014(4) -0.0003(4) N1 0.0173(6) 0.0187(6) 0.0130(5) 0.0009(4) 0.0008(4) 0.0011(5) N2 0.0159(5) 0.0145(5) 0.0134(5) -0.0002(4) 0.0006(4) 0.0000(4) N3 0.0158(6) 0.0259(6) 0.0140(5) -0.0009(5) -0.0003(4) 0.0032(5) N4 0.0162(6) 0.0243(6) 0.0181(6) 0.0004(5) 0.0019(5) 0.0024(5) C1 0.0188(7) 0.0169(7) 0.0184(7) -0.0012(5) 0.0008(5) 0.0018(5) C2 0.0174(7) 0.0207(7) 0.0169(7) -0.0010(5) 0.0035(5) 0.0019(5) C3 0.0188(7) 0.0149(6) 0.0133(6) -0.0029(5) 0.0018(5) -0.0023(5) C4 0.0210(7) 0.0345(9) 0.0200(7) 0.0045(6) 0.0031(6) 0.0084(6) C5 0.0182(7) 0.0235(7) 0.0178(7) 0.0017(6) 0.0039(5) 0.0006(6) C6 0.0167(7) 0.0271(8) 0.0147(6) 0.0035(6) 0.0019(5) 0.0046(6) C7 0.0163(7) 0.0314(8) 0.0180(7) 0.0009(6) 0.0006(5) 0.0041(6) C8 0.0267(8) 0.0416(9) 0.0161(7) -0.0012(6) 0.0009(6) 0.0074(7) C9 0.0377(9) 0.0459(10) 0.0150(7) 0.0090(7) 0.0071(6) 0.0143(8) C10 0.0371(9) 0.0313(9) 0.0228(8) 0.0099(6) 0.0109(7) 0.0107(7) C11 0.0246(7) 0.0268(8) 0.0207(7) 0.0055(6) 0.0063(6) 0.0077(6) C12 0.0264(8) 0.0316(8) 0.0160(7) -0.0044(6) 0.0003(6) -0.0047(6) C13 0.0291(9) 0.0513(11) 0.0283(8) -0.0095(8) 0.0024(7) -0.0106(8) C14 0.0351(9) 0.0290(8) 0.0245(8) -0.0036(6) 0.0004(7) -0.0029(7) C15 0.0387(9) 0.0220(8) 0.0231(7) 0.0068(6) 0.0067(6) 0.0017(7) C16 0.0627(12) 0.0248(9) 0.0321(9) 0.0053(7) 0.0092(8) 0.0104(8) C17 0.0475(11) 0.0336(9) 0.0366(9) 0.0068(7) 0.0082(8) -0.0102(8) C18 0.0143(6) 0.0160(6) 0.0158(6) 0.0034(5) 0.0032(5) -0.0001(5) C19 0.0155(6) 0.0176(7) 0.0184(7) 0.0002(5) 0.0036(5) -0.0007(5) C20 0.0210(7) 0.0158(7) 0.0251(7) 0.0008(6) 0.0055(6) 0.0014(5) C21 0.0202(7) 0.0209(7) 0.0228(7) 0.0075(6) 0.0008(6) 0.0023(6) C22 0.0196(7) 0.0228(7) 0.0175(7) 0.0032(6) -0.0004(5) -0.0016(6) C23 0.0158(6) 0.0181(7) 0.0162(6) 0.0017(5) 0.0033(5) -0.0019(5) C24 0.0204(7) 0.0164(7) 0.0191(7) -0.0018(5) 0.0010(5) 0.0005(5) C25 0.0247(8) 0.0317(8) 0.0238(7) -0.0003(6) 0.0001(6) -0.0066(6) C26 0.0357(9) 0.0424(10) 0.0337(9) -0.0189(8) -0.0062(7) 0.0156(8) C27 0.0209(7) 0.0178(7) 0.0144(6) 0.0001(5) -0.0002(5) -0.0007(5) C28 0.0302(8) 0.0261(8) 0.0173(7) -0.0020(6) 0.0035(6) -0.0036(6) C29 0.0232(7) 0.0194(7) 0.0211(7) -0.0022(6) -0.0004(6) -0.0025(6) C31 0.0171(6) 0.0153(6) 0.0171(6) 0.0008(5) 0.0039(5) -0.0024(5) C32 0.0170(7) 0.0138(6) 0.0220(7) 0.0001(5) 0.0008(5) -0.0030(5) C33 0.0206(7) 0.0244(7) 0.0210(7) 0.0019(6) 0.0029(6) -0.0013(6) C34 0.0172(7) 0.0269(8) 0.0312(8) -0.0004(6) 0.0066(6) -0.0008(6) C35 0.0168(7) 0.0211(7) 0.0336(8) -0.0001(6) -0.0032(6) 0.0011(6) C36 0.0254(7) 0.0201(7) 0.0225(7) 0.0007(6) -0.0036(6) 0.0000(6) C37 0.0206(7) 0.0175(7) 0.0210(7) -0.0006(5) 0.0014(5) -0.0002(5) C38 0.0356(9) 0.0337(9) 0.0249(8) -0.0067(7) -0.0017(7) 0.0056(7) C39 0.0438(10) 0.0327(9) 0.0238(8) -0.0039(7) -0.0033(7) 0.0048(7) C40 0.0526(13) 0.0316(10) 0.0203(9) -0.0032(7) -0.0016(8) -0.0077(9) C37' 0.0356(9) 0.0337(9) 0.0249(8) -0.0067(7) -0.0017(7) 0.0056(7) C38' 0.0438(10) 0.0327(9) 0.0238(8) -0.0039(7) -0.0033(7) 0.0048(7) C39' 0.0526(13) 0.0316(10) 0.0203(9) -0.0032(7) -0.0016(8) -0.0077(9) C40' 0.024(4) 0.024(3) 0.025(3) 0.009(3) -0.001(2) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N3 1.7391(12) . ? Si1 O1 1.7667(10) . ? Si1 N2 1.8371(11) . ? Si1 N1 1.9437(12) . ? Si1 H1S 1.376(15) . ? O1 C31 1.3395(16) . ? N1 C1 1.3246(17) . ? N1 C6 1.4532(17) . ? N2 C3 1.3512(17) . ? N2 C18 1.4578(16) . ? N3 N4 1.4021(16) . ? N3 H3N 0.8800 . ? N4 C31 1.2873(17) . ? C1 C2 1.4005(19) . ? C1 C4 1.5098(19) . ? C2 C3 1.3847(19) . ? C2 H2 0.943(16) . ? C3 C5 1.5087(18) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C4 H4D 0.9800 . ? C4 H4E 0.9800 . ? C4 H4F 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.402(2) . ? C6 C7 1.405(2) . ? C7 C8 1.398(2) . ? C7 C12 1.523(2) . ? C8 C9 1.380(2) . ? C8 H8 0.9500 . ? C9 C10 1.377(2) . ? C9 H9 0.9500 . ? C10 C11 1.395(2) . ? C10 H10 0.9500 . ? C11 C15 1.522(2) . ? C12 C13 1.533(2) . ? C12 C14 1.536(2) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.532(2) . ? C15 C16 1.535(2) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.4029(19) . ? C18 C23 1.4042(18) . ? C19 C20 1.3975(19) . ? C19 C24 1.5243(19) . ? C20 C21 1.384(2) . ? C20 H20 0.9500 . ? C21 C22 1.385(2) . ? C21 H21 0.9500 . ? C22 C23 1.3961(19) . ? C22 H22 0.9500 . ? C23 C27 1.5262(19) . ? C24 C26 1.522(2) . ? C24 C25 1.530(2) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.5342(19) . ? C27 C28 1.5370(18) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C32 1.4693(19) . ? C32 C37 1.3924(19) . ? C32 C33 1.3980(19) . ? C33 C34 1.386(2) . ? C33 H33 0.9500 . ? C34 C35 1.388(2) . ? C34 H34 0.9500 . ? C35 C36 1.385(2) . ? C35 H35 0.9500 . ? C36 C37 1.389(2) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.520(2) . ? C38 C38 1.524(3) 3_665 ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.521(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C40' H40D 0.9800 . ? C40' H40E 0.9800 . ? C40' H40F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Si1 O1 83.70(5) . . ? N3 Si1 N2 128.58(6) . . ? O1 Si1 N2 90.88(5) . . ? N3 Si1 N1 89.33(5) . . ? O1 Si1 N1 172.69(5) . . ? N2 Si1 N1 91.74(5) . . ? N3 Si1 H1S 126.5(6) . . ? O1 Si1 H1S 94.6(6) . . ? N2 Si1 H1S 104.9(6) . . ? N1 Si1 H1S 91.3(6) . . ? C31 O1 Si1 112.89(8) . . ? C1 N1 C6 117.05(11) . . ? C1 N1 Si1 121.98(9) . . ? C6 N1 Si1 119.75(9) . . ? C3 N2 C18 116.43(11) . . ? C3 N2 Si1 123.50(9) . . ? C18 N2 Si1 119.11(8) . . ? N4 N3 Si1 117.74(9) . . ? N4 N3 H3N 121.1 . . ? Si1 N3 H3N 121.1 . . ? C31 N4 N3 106.64(11) . . ? N1 C1 C2 121.77(12) . . ? N1 C1 C4 121.33(12) . . ? C2 C1 C4 116.84(12) . . ? C3 C2 C1 124.53(13) . . ? C3 C2 H2 118.6(10) . . ? C1 C2 H2 115.6(10) . . ? N2 C3 C2 123.06(12) . . ? N2 C3 C5 119.65(12) . . ? C2 C3 C5 117.26(12) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 C4 H4D 109.5 . . ? H4A C4 H4D 141.1 . . ? H4B C4 H4D 56.3 . . ? H4C C4 H4D 56.3 . . ? C1 C4 H4E 109.5 . . ? H4A C4 H4E 56.3 . . ? H4B C4 H4E 141.1 . . ? H4C C4 H4E 56.3 . . ? H4D C4 H4E 109.5 . . ? C1 C4 H4F 109.5 . . ? H4A C4 H4F 56.3 . . ? H4B C4 H4F 56.3 . . ? H4C C4 H4F 141.1 . . ? H4D C4 H4F 109.5 . . ? H4E C4 H4F 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 121.66(13) . . ? C11 C6 N1 119.08(12) . . ? C7 C6 N1 119.25(12) . . ? C8 C7 C6 118.08(14) . . ? C8 C7 C12 119.26(13) . . ? C6 C7 C12 122.66(12) . . ? C9 C8 C7 120.87(15) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 120.12(14) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 121.56(15) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 117.68(14) . . ? C10 C11 C15 119.53(14) . . ? C6 C11 C15 122.78(13) . . ? C7 C12 C13 110.43(13) . . ? C7 C12 C14 112.14(12) . . ? C13 C12 C14 109.77(13) . . ? C7 C12 H12 108.1 . . ? C13 C12 H12 108.1 . . ? C14 C12 H12 108.1 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 110.53(13) . . ? C11 C15 C16 111.77(13) . . ? C17 C15 C16 110.98(14) . . ? C11 C15 H15 107.8 . . ? C17 C15 H15 107.8 . . ? C16 C15 H15 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 122.04(12) . . ? C19 C18 N2 117.82(11) . . ? C23 C18 N2 120.15(12) . . ? C20 C19 C18 117.83(12) . . ? C20 C19 C24 121.26(12) . . ? C18 C19 C24 120.91(12) . . ? C21 C20 C19 121.16(13) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 119.89(13) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 121.37(13) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C18 117.65(13) . . ? C22 C23 C27 118.96(12) . . ? C18 C23 C27 123.31(12) . . ? C26 C24 C19 112.77(12) . . ? C26 C24 C25 110.81(13) . . ? C19 C24 C25 111.83(11) . . ? C26 C24 H24 107.0 . . ? C19 C24 H24 107.0 . . ? C25 C24 H24 107.0 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 110.66(11) . . ? C23 C27 C28 112.86(11) . . ? C29 C27 C28 108.52(11) . . ? C23 C27 H27 108.2 . . ? C29 C27 H27 108.2 . . ? C28 C27 H27 108.2 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N4 C31 O1 118.74(12) . . ? N4 C31 C32 122.80(12) . . ? O1 C31 C32 118.40(11) . . ? C37 C32 C33 119.24(13) . . ? C37 C32 C31 119.51(12) . . ? C33 C32 C31 121.23(12) . . ? C34 C33 C32 120.07(13) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.37(14) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C36 C35 C34 119.78(13) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 120.18(14) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C32 120.33(13) . . ? C36 C37 H37 119.8 . . ? C32 C37 H37 119.8 . . ? C39 C38 C38 114.78(17) . 3_665 ? C39 C38 H38A 108.6 . . ? C38 C38 H38A 108.6 3_665 . ? C39 C38 H38B 108.6 . . ? C38 C38 H38B 108.6 3_665 . ? H38A C38 H38B 107.5 . . ? C38 C39 C40 113.12(14) . . ? C38 C39 H39A 109.0 . . ? C40 C39 H39A 109.0 . . ? C38 C39 H39B 109.0 . . ? C40 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? H40D C40' H40E 109.5 . . ? H40D C40' H40F 109.5 . . ? H40E C40' H40F 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 N3 Si1 O1 C31 -4.71(9) . . . . ? N2 Si1 O1 C31 124.03(9) . . . . ? N1 Si1 O1 C31 13.0(4) . . . . ? N3 Si1 N1 C1 164.69(11) . . . . ? O1 Si1 N1 C1 147.1(4) . . . . ? N2 Si1 N1 C1 36.11(11) . . . . ? N3 Si1 N1 C6 -28.27(11) . . . . ? O1 Si1 N1 C6 -45.9(4) . . . . ? N2 Si1 N1 C6 -156.85(10) . . . . ? N3 Si1 N2 C3 -123.86(10) . . . . ? O1 Si1 N2 C3 153.49(10) . . . . ? N1 Si1 N2 C3 -33.33(11) . . . . ? N3 Si1 N2 C18 67.74(11) . . . . ? O1 Si1 N2 C18 -14.90(10) . . . . ? N1 Si1 N2 C18 158.27(9) . . . . ? O1 Si1 N3 N4 4.58(10) . . . . ? N2 Si1 N3 N4 -81.52(11) . . . . ? N1 Si1 N3 N4 -173.20(10) . . . . ? Si1 N3 N4 C31 -3.24(14) . . . . ? C6 N1 C1 C2 173.05(13) . . . . ? Si1 N1 C1 C2 -19.58(18) . . . . ? C6 N1 C1 C4 -3.95(19) . . . . ? Si1 N1 C1 C4 163.41(11) . . . . ? N1 C1 C2 C3 -11.7(2) . . . . ? C4 C1 C2 C3 165.41(14) . . . . ? C18 N2 C3 C2 -176.56(12) . . . . ? Si1 N2 C3 C2 14.76(18) . . . . ? C18 N2 C3 C5 1.41(17) . . . . ? Si1 N2 C3 C5 -167.27(9) . . . . ? C1 C2 C3 N2 15.3(2) . . . . ? C1 C2 C3 C5 -162.69(13) . . . . ? C1 N1 C6 C11 88.30(16) . . . . ? Si1 N1 C6 C11 -79.36(14) . . . . ? C1 N1 C6 C7 -92.74(16) . . . . ? Si1 N1 C6 C7 99.60(13) . . . . ? C11 C6 C7 C8 1.3(2) . . . . ? N1 C6 C7 C8 -177.68(12) . . . . ? C11 C6 C7 C12 -177.92(13) . . . . ? N1 C6 C7 C12 3.1(2) . . . . ? C6 C7 C8 C9 -1.6(2) . . . . ? C12 C7 C8 C9 177.60(14) . . . . ? C7 C8 C9 C10 0.7(2) . . . . ? C8 C9 C10 C11 0.7(2) . . . . ? C9 C10 C11 C6 -1.0(2) . . . . ? C9 C10 C11 C15 178.38(15) . . . . ? C7 C6 C11 C10 0.0(2) . . . . ? N1 C6 C11 C10 178.97(13) . . . . ? C7 C6 C11 C15 -179.36(13) . . . . ? N1 C6 C11 C15 -0.4(2) . . . . ? C8 C7 C12 C13 -63.60(17) . . . . ? C6 C7 C12 C13 115.57(15) . . . . ? C8 C7 C12 C14 59.16(18) . . . . ? C6 C7 C12 C14 -121.67(14) . . . . ? C10 C11 C15 C17 -72.89(18) . . . . ? C6 C11 C15 C17 106.49(16) . . . . ? C10 C11 C15 C16 51.25(19) . . . . ? C6 C11 C15 C16 -129.37(15) . . . . ? C3 N2 C18 C19 104.14(14) . . . . ? Si1 N2 C18 C19 -86.66(13) . . . . ? C3 N2 C18 C23 -75.81(15) . . . . ? Si1 N2 C18 C23 93.39(13) . . . . ? C23 C18 C19 C20 2.93(19) . . . . ? N2 C18 C19 C20 -177.02(11) . . . . ? C23 C18 C19 C24 -176.59(12) . . . . ? N2 C18 C19 C24 3.46(18) . . . . ? C18 C19 C20 C21 -1.0(2) . . . . ? C24 C19 C20 C21 178.51(13) . . . . ? C19 C20 C21 C22 -0.8(2) . . . . ? C20 C21 C22 C23 0.9(2) . . . . ? C21 C22 C23 C18 1.0(2) . . . . ? C21 C22 C23 C27 -176.01(12) . . . . ? C19 C18 C23 C22 -2.90(19) . . . . ? N2 C18 C23 C22 177.04(12) . . . . ? C19 C18 C23 C27 173.93(12) . . . . ? N2 C18 C23 C27 -6.13(19) . . . . ? C20 C19 C24 C26 -28.48(19) . . . . ? C18 C19 C24 C26 151.03(14) . . . . ? C20 C19 C24 C25 97.19(15) . . . . ? C18 C19 C24 C25 -83.30(16) . . . . ? C22 C23 C27 C29 69.10(15) . . . . ? C18 C23 C27 C29 -107.69(14) . . . . ? C22 C23 C27 C28 -52.73(17) . . . . ? C18 C23 C27 C28 130.47(13) . . . . ? N3 N4 C31 O1 -0.82(16) . . . . ? N3 N4 C31 C32 176.42(12) . . . . ? Si1 O1 C31 N4 4.34(15) . . . . ? Si1 O1 C31 C32 -173.01(9) . . . . ? N4 C31 C32 C37 -158.32(13) . . . . ? O1 C31 C32 C37 18.92(19) . . . . ? N4 C31 C32 C33 19.8(2) . . . . ? O1 C31 C32 C33 -163.00(12) . . . . ? C37 C32 C33 C34 1.1(2) . . . . ? C31 C32 C33 C34 -177.03(13) . . . . ? C32 C33 C34 C35 0.5(2) . . . . ? C33 C34 C35 C36 -1.5(2) . . . . ? C34 C35 C36 C37 0.9(2) . . . . ? C35 C36 C37 C32 0.6(2) . . . . ? C33 C32 C37 C36 -1.6(2) . . . . ? C31 C32 C37 C36 176.50(13) . . . . ? C38 C38 C39 C40 -179.66(18) 3_665 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.306 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.041 data_p212121 _database_code_depnum_ccdc_archive 'CCDC 843520' #TrackingRef '7081_web_deposit_cif_file_0_JakobHey_1315469731.p212121_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H48 N4 O2 Si' _chemical_formula_sum 'C33 H48 N4 O2 Si' _chemical_formula_weight 560.84 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' 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' _cell_length_a 13.816(2) _cell_length_b 14.387(2) _cell_length_c 15.751(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3130.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9893 _cell_measurement_theta_min 2.419 _cell_measurement_theta_max 27.082 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9891 _exptl_absorpt_correction_T_max 0.9956 _exptl_absorpt_process_details 'SADABS 2008/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC I\mS microfocus source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Bruker APEX II with D8' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26322 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.13 _reflns_number_total 6906 _reflns_number_gt 6198 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.11-3' _computing_cell_refinement 'SAINT V7.60A' _computing_data_reduction 'SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XSHELL in SHELXTL-97' _computing_publication_material 'XSHELL in SHELXTL-97' _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^)+(0.0521P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(8) _refine_ls_number_reflns 6906 _refine_ls_number_parameters 379 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si3 Si 0.35314(3) 0.34990(3) 0.21413(3) 0.01333(10) Uani 1 1 d D . . H3S H 0.4250(11) 0.3078(11) 0.1565(10) 0.016 Uiso 1 1 d D . . O1 O 0.33456(8) 0.34437(8) 0.32140(7) 0.0176(2) Uani 1 1 d . . . O2 O 0.30367(9) 0.19594(8) 0.07689(8) 0.0237(3) Uani 1 1 d . . . N1 N 0.44722(9) 0.44530(9) 0.23725(8) 0.0141(3) Uani 1 1 d . . . N2 N 0.26613(9) 0.42989(9) 0.16960(8) 0.0152(3) Uani 1 1 d . . . N3 N 0.28007(9) 0.24156(9) 0.21214(9) 0.0161(3) Uani 1 1 d . . . N4 N 0.24985(10) 0.21151(9) 0.29317(9) 0.0186(3) Uani 1 1 d . . . C1 C 0.54732(12) 0.41384(11) 0.24011(10) 0.0175(3) Uani 1 1 d . . . C2 C 0.58764(12) 0.37940(11) 0.31603(11) 0.0213(4) Uani 1 1 d . . . C3 C 0.68185(13) 0.34368(12) 0.31229(12) 0.0260(4) Uani 1 1 d . . . H3 H 0.7105 0.3193 0.3624 0.031 Uiso 1 1 calc R . . C4 C 0.73377(13) 0.34305(13) 0.23812(13) 0.0306(4) Uani 1 1 d . . . H4 H 0.7972 0.3176 0.2372 0.037 Uiso 1 1 calc R . . C5 C 0.69427(13) 0.37919(12) 0.16493(13) 0.0271(4) Uani 1 1 d . . . H5 H 0.7313 0.3791 0.1141 0.033 Uiso 1 1 calc R . . C6 C 0.60078(12) 0.41594(11) 0.16422(11) 0.0202(4) Uani 1 1 d . . . C7 C 0.56229(12) 0.45730(11) 0.08169(11) 0.0206(4) Uani 1 1 d . . . H7 H 0.4944 0.4787 0.0918 0.025 Uiso 1 1 calc R . . C8 C 0.62273(14) 0.54138(13) 0.05471(13) 0.0311(4) Uani 1 1 d . . . H8A H 0.5932 0.5705 0.0048 0.047 Uiso 1 1 calc R . . H8B H 0.6885 0.5211 0.0407 0.047 Uiso 1 1 calc R . . H8C H 0.6252 0.5864 0.1013 0.047 Uiso 1 1 calc R . . C9 C 0.56061(14) 0.38495(13) 0.01067(11) 0.0266(4) Uani 1 1 d . . . H9A H 0.5390 0.4143 -0.0422 0.040 Uiso 1 1 calc R . . H9B H 0.5160 0.3347 0.0259 0.040 Uiso 1 1 calc R . . H9C H 0.6258 0.3595 0.0028 0.040 Uiso 1 1 calc R . . C10 C 0.53626(13) 0.38093(12) 0.40129(11) 0.0242(4) Uani 1 1 d . . . H10 H 0.4712 0.4100 0.3931 0.029 Uiso 1 1 calc R . . C11 C 0.52135(15) 0.28157(13) 0.43417(13) 0.0328(5) Uani 1 1 d . . . H11A H 0.4876 0.2836 0.4889 0.049 Uiso 1 1 calc R . . H11B H 0.5844 0.2513 0.4414 0.049 Uiso 1 1 calc R . . H11C H 0.4825 0.2463 0.3932 0.049 Uiso 1 1 calc R . . C12 C 0.59233(14) 0.43893(13) 0.46654(12) 0.0302(4) Uani 1 1 d . . . H12A H 0.5557 0.4415 0.5198 0.045 Uiso 1 1 calc R . . H12B H 0.6015 0.5021 0.4446 0.045 Uiso 1 1 calc R . . H12C H 0.6556 0.4103 0.4770 0.045 Uiso 1 1 calc R . . C13 C 0.42877(12) 0.53459(11) 0.24708(10) 0.0158(3) Uani 1 1 d . . . C14 C 0.50648(12) 0.60146(11) 0.27474(10) 0.0190(3) Uani 1 1 d . . . H14A H 0.4781 0.6632 0.2833 0.028 Uiso 1 1 calc R . . H14B H 0.5566 0.6050 0.2309 0.028 Uiso 1 1 calc R . . H14C H 0.5353 0.5797 0.3280 0.028 Uiso 1 1 calc R . . C15 C 0.33693(12) 0.57078(11) 0.22728(10) 0.0175(3) Uani 1 1 d D . . H15 H 0.3268(13) 0.6360(10) 0.2363(11) 0.021 Uiso 1 1 d D . . C16 C 0.26517(12) 0.52332(11) 0.18482(10) 0.0165(3) Uani 1 1 d . . . C17 C 0.18229(13) 0.58140(12) 0.15112(12) 0.0227(4) Uani 1 1 d . . . H17A H 0.1924 0.6466 0.1666 0.034 Uiso 1 1 calc R . . H17B H 0.1213 0.5594 0.1758 0.034 Uiso 1 1 calc R . . H17C H 0.1795 0.5757 0.0892 0.034 Uiso 1 1 calc R . . C18 C 0.18694(12) 0.39469(11) 0.11631(11) 0.0165(3) Uani 1 1 d . . . C19 C 0.20386(12) 0.38502(11) 0.02891(11) 0.0183(3) Uani 1 1 d . . . C20 C 0.12501(13) 0.36358(12) -0.02296(11) 0.0237(4) Uani 1 1 d . . . H20 H 0.1346 0.3574 -0.0824 0.028 Uiso 1 1 calc R . . C21 C 0.03322(13) 0.35118(12) 0.01035(11) 0.0256(4) Uani 1 1 d . . . H21 H -0.0200 0.3389 -0.0262 0.031 Uiso 1 1 calc R . . C22 C 0.01948(12) 0.35670(12) 0.09683(11) 0.0237(4) Uani 1 1 d . . . H22 H -0.0433 0.3459 0.1194 0.028 Uiso 1 1 calc R . . C23 C 0.09547(12) 0.37774(11) 0.15236(11) 0.0192(4) Uani 1 1 d . . . C24 C 0.30397(13) 0.39883(11) -0.00974(10) 0.0192(4) Uani 1 1 d . . . H24 H 0.3527 0.3830 0.0349 0.023 Uiso 1 1 calc R . . C25 C 0.32250(13) 0.33495(13) -0.08571(11) 0.0259(4) Uani 1 1 d . . . H25A H 0.3907 0.3392 -0.1024 0.039 Uiso 1 1 calc R . . H25B H 0.2814 0.3540 -0.1333 0.039 Uiso 1 1 calc R . . H25C H 0.3073 0.2707 -0.0700 0.039 Uiso 1 1 calc R . . C26 C 0.32027(15) 0.50029(12) -0.03486(12) 0.0283(4) Uani 1 1 d . . . H26A H 0.3833 0.5064 -0.0628 0.042 Uiso 1 1 calc R . . H26B H 0.3189 0.5394 0.0161 0.042 Uiso 1 1 calc R . . H26C H 0.2691 0.5201 -0.0739 0.042 Uiso 1 1 calc R . . C27 C 0.07405(13) 0.37863(13) 0.24762(11) 0.0246(4) Uani 1 1 d . . . H27 H 0.1361 0.3902 0.2786 0.029 Uiso 1 1 calc R . . C28 C 0.03390(13) 0.28390(14) 0.27582(13) 0.0328(5) Uani 1 1 d . . . H28A H 0.0317 0.2813 0.3380 0.049 Uiso 1 1 calc R . . H28B H 0.0759 0.2343 0.2545 0.049 Uiso 1 1 calc R . . H28C H -0.0315 0.2757 0.2530 0.049 Uiso 1 1 calc R . . C29 C 0.00165(14) 0.45400(14) 0.27302(12) 0.0324(4) Uani 1 1 d . . . H29A H -0.0163 0.4460 0.3328 0.049 Uiso 1 1 calc R . . H29B H -0.0563 0.4490 0.2375 0.049 Uiso 1 1 calc R . . H29C H 0.0311 0.5153 0.2651 0.049 Uiso 1 1 calc R . . C30 C 0.28010(12) 0.27049(11) 0.34735(11) 0.0193(4) Uani 1 1 d . . . C31 C 0.25805(14) 0.26356(13) 0.43925(11) 0.0279(4) Uani 1 1 d . . . H31A H 0.2266 0.2039 0.4509 0.042 Uiso 1 1 calc R . . H31B H 0.2147 0.3144 0.4557 0.042 Uiso 1 1 calc R . . H31C H 0.3183 0.2679 0.4719 0.042 Uiso 1 1 calc R . . C32 C 0.27352(12) 0.17743(11) 0.14865(11) 0.0181(3) Uani 1 1 d . . . C33 C 0.22897(13) 0.08445(12) 0.16924(12) 0.0256(4) Uani 1 1 d . . . H33A H 0.1631 0.0937 0.1908 0.038 Uiso 1 1 calc R . . H33B H 0.2681 0.0530 0.2125 0.038 Uiso 1 1 calc R . . H33C H 0.2267 0.0462 0.1178 0.038 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 Si3 0.0107(2) 0.0139(2) 0.0154(2) 0.00092(17) -0.00044(17) -0.00030(16) O1 0.0179(6) 0.0178(5) 0.0169(5) 0.0020(5) 0.0001(4) -0.0025(5) O2 0.0233(7) 0.0248(6) 0.0231(7) -0.0024(5) -0.0019(5) 0.0001(5) N1 0.0102(6) 0.0170(6) 0.0152(6) 0.0012(5) -0.0002(5) -0.0007(5) N2 0.0106(7) 0.0165(6) 0.0184(7) 0.0012(5) -0.0017(5) 0.0007(5) N3 0.0132(7) 0.0160(6) 0.0191(7) 0.0014(6) 0.0003(6) 0.0001(5) N4 0.0153(7) 0.0185(7) 0.0220(7) 0.0050(6) 0.0030(6) 0.0004(5) C1 0.0124(8) 0.0133(7) 0.0268(9) -0.0025(6) -0.0032(7) -0.0015(6) C2 0.0178(9) 0.0151(8) 0.0309(9) -0.0008(7) -0.0056(7) -0.0036(7) C3 0.0197(9) 0.0183(8) 0.0399(11) -0.0015(8) -0.0110(8) 0.0023(7) C4 0.0138(8) 0.0223(9) 0.0558(13) -0.0053(9) -0.0061(8) 0.0026(7) C5 0.0167(9) 0.0229(9) 0.0417(11) -0.0061(8) 0.0038(8) -0.0007(7) C6 0.0139(8) 0.0156(8) 0.0311(9) -0.0038(7) 0.0004(7) -0.0021(6) C7 0.0160(8) 0.0222(8) 0.0237(9) -0.0010(7) 0.0060(7) 0.0013(7) C8 0.0340(11) 0.0280(10) 0.0314(10) -0.0033(8) 0.0082(9) -0.0036(8) C9 0.0223(10) 0.0285(9) 0.0291(10) -0.0035(8) 0.0052(8) -0.0028(8) C10 0.0213(9) 0.0254(9) 0.0259(9) 0.0032(7) -0.0083(7) 0.0004(7) C11 0.0325(11) 0.0328(10) 0.0331(10) 0.0087(9) -0.0099(9) -0.0051(8) C12 0.0323(11) 0.0290(10) 0.0293(10) -0.0007(8) -0.0116(8) 0.0026(8) C13 0.0152(8) 0.0197(8) 0.0124(7) 0.0015(6) 0.0034(6) -0.0006(6) C14 0.0197(9) 0.0160(7) 0.0213(9) -0.0015(7) -0.0006(7) -0.0014(6) C15 0.0194(9) 0.0149(7) 0.0180(8) -0.0016(6) 0.0020(7) 0.0020(6) C16 0.0142(8) 0.0179(8) 0.0174(8) 0.0015(6) 0.0036(6) 0.0021(6) C17 0.0189(9) 0.0173(8) 0.0319(10) 0.0021(7) -0.0036(7) 0.0034(7) C18 0.0136(8) 0.0145(7) 0.0214(8) 0.0005(6) -0.0061(7) 0.0001(6) C19 0.0188(9) 0.0157(8) 0.0205(8) 0.0027(6) -0.0030(7) 0.0021(7) C20 0.0261(10) 0.0223(9) 0.0229(8) -0.0016(7) -0.0078(7) 0.0013(7) C21 0.0214(9) 0.0228(8) 0.0325(10) -0.0020(8) -0.0128(8) 0.0004(7) C22 0.0129(8) 0.0242(9) 0.0340(10) -0.0014(8) -0.0036(7) 0.0007(7) C23 0.0150(9) 0.0179(8) 0.0246(9) 0.0017(7) -0.0018(7) 0.0023(6) C24 0.0196(9) 0.0222(8) 0.0157(8) -0.0007(7) -0.0022(7) -0.0010(7) C25 0.0256(10) 0.0317(10) 0.0206(9) -0.0025(8) -0.0017(7) 0.0041(8) C26 0.0323(11) 0.0278(10) 0.0247(9) 0.0027(8) 0.0065(8) -0.0005(8) C27 0.0135(9) 0.0350(10) 0.0252(9) 0.0006(8) -0.0018(7) -0.0014(7) C28 0.0163(9) 0.0425(11) 0.0397(11) 0.0111(10) 0.0033(8) -0.0001(8) C29 0.0247(10) 0.0389(11) 0.0336(11) -0.0066(9) 0.0040(9) -0.0029(8) C30 0.0180(9) 0.0174(8) 0.0224(9) 0.0028(7) 0.0041(7) 0.0025(7) C31 0.0386(11) 0.0236(9) 0.0214(9) 0.0030(7) 0.0095(8) 0.0024(8) C32 0.0121(8) 0.0166(8) 0.0257(9) 0.0011(7) -0.0061(7) 0.0014(6) C33 0.0241(10) 0.0191(9) 0.0336(10) -0.0024(8) -0.0059(8) -0.0024(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si3 O1 1.7109(12) . ? Si3 N2 1.8059(14) . ? Si3 N3 1.8573(14) . ? Si3 N1 1.9250(14) . ? O1 C30 1.365(2) . ? O2 C32 1.234(2) . ? N1 C13 1.319(2) . ? N1 C1 1.456(2) . ? N2 C16 1.366(2) . ? N2 C18 1.469(2) . ? N3 C32 1.364(2) . ? N3 N4 1.4107(19) . ? N4 C30 1.274(2) . ? C1 C6 1.405(2) . ? C1 C2 1.409(2) . ? C2 C3 1.401(2) . ? C2 C10 1.519(3) . ? C3 C4 1.371(3) . ? C4 C5 1.377(3) . ? C5 C6 1.396(2) . ? C6 C7 1.525(2) . ? C7 C9 1.528(2) . ? C7 C8 1.530(2) . ? C10 C12 1.534(2) . ? C10 C11 1.534(2) . ? C13 C15 1.406(2) . ? C13 C14 1.506(2) . ? C15 C16 1.377(2) . ? C16 C17 1.514(2) . ? C18 C19 1.403(2) . ? C18 C23 1.407(2) . ? C19 C20 1.396(2) . ? C19 C24 1.524(2) . ? C20 C21 1.384(3) . ? C21 C22 1.378(3) . ? C22 C23 1.400(2) . ? C23 C27 1.530(2) . ? C24 C26 1.529(2) . ? C24 C25 1.530(2) . ? C27 C29 1.529(3) . ? C27 C28 1.537(3) . ? C30 C31 1.483(2) . ? C32 C33 1.508(2) . ? 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 O1 Si3 N2 108.26(6) . . ? O1 Si3 N3 84.03(6) . . ? N2 Si3 N3 99.58(6) . . ? O1 Si3 N1 87.00(6) . . ? N2 Si3 N1 93.94(6) . . ? N3 Si3 N1 165.58(6) . . ? C30 O1 Si3 114.50(10) . . ? C13 N1 C1 118.87(13) . . ? C13 N1 Si3 125.89(11) . . ? C1 N1 Si3 115.19(10) . . ? C16 N2 C18 115.63(13) . . ? C16 N2 Si3 124.44(11) . . ? C18 N2 Si3 119.87(10) . . ? C32 N3 N4 115.87(13) . . ? C32 N3 Si3 128.04(12) . . ? N4 N3 Si3 113.76(10) . . ? C30 N4 N3 107.74(13) . . ? C6 C1 C2 121.43(15) . . ? C6 C1 N1 117.79(14) . . ? C2 C1 N1 120.74(15) . . ? C3 C2 C1 117.44(17) . . ? C3 C2 C10 118.47(16) . . ? C1 C2 C10 124.07(15) . . ? C4 C3 C2 121.63(17) . . ? C3 C4 C5 120.23(17) . . ? C4 C5 C6 121.08(18) . . ? C5 C6 C1 118.13(16) . . ? C5 C6 C7 118.50(16) . . ? C1 C6 C7 123.37(15) . . ? C6 C7 C9 111.31(14) . . ? C6 C7 C8 110.79(15) . . ? C9 C7 C8 110.09(14) . . ? C2 C10 C12 111.36(15) . . ? C2 C10 C11 110.34(15) . . ? C12 C10 C11 110.39(15) . . ? N1 C13 C15 120.59(15) . . ? N1 C13 C14 121.23(14) . . ? C15 C13 C14 118.08(14) . . ? C16 C15 C13 125.00(15) . . ? N2 C16 C15 124.50(15) . . ? N2 C16 C17 119.29(14) . . ? C15 C16 C17 116.19(15) . . ? C19 C18 C23 121.89(15) . . ? C19 C18 N2 118.08(14) . . ? C23 C18 N2 119.89(14) . . ? C20 C19 C18 117.78(16) . . ? C20 C19 C24 120.21(15) . . ? C18 C19 C24 122.00(15) . . ? C21 C20 C19 121.44(17) . . ? C22 C21 C20 119.58(16) . . ? C21 C22 C23 121.81(17) . . ? C22 C23 C18 117.34(15) . . ? C22 C23 C27 118.03(15) . . ? C18 C23 C27 124.62(15) . . ? C19 C24 C26 111.19(14) . . ? C19 C24 C25 112.69(14) . . ? C26 C24 C25 110.26(14) . . ? C29 C27 C23 112.91(15) . . ? C29 C27 C28 108.49(15) . . ? C23 C27 C28 110.23(15) . . ? N4 C30 O1 119.93(15) . . ? N4 C30 C31 122.81(16) . . ? O1 C30 C31 117.26(15) . . ? O2 C32 N3 120.22(15) . . ? O2 C32 C33 121.76(15) . . ? N3 C32 C33 118.01(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.13 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.324 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.047