_publ_contact_author 'Anton V. Cherkasov' _publ_contact_author_email 'ach@iomc.ras.ru' _publ_author_name 'L. Luconi, D. Lyubov, A. Rossin, A. Cherkasov, G. Tuci, G. Fukin, A. Trifonov, G. Giambastiani' _journal_name_full 'Organometallics' data_lunnn _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H52 Lu N3 S Si2' _chemical_formula_weight 741.98 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Lu' 'Lu' -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'Pn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 9.36415(7) _cell_length_b 11.51241(8) _cell_length_c 16.74418(12) _cell_angle_alpha 90.00 _cell_angle_beta 92.3218(7) _cell_angle_gamma 90.00 _cell_volume 1803.61(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24638 _cell_measurement_theta_min 3.0040 _cell_measurement_theta_max 32.3825 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 2.884 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.4782 _exptl_absorpt_correction_T_max 0.5962 _exptl_absorpt_process_details ; SCALE3 ABSPACK, CrysAlisPro, Agilent Technologies (2012) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31271 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 28.00 _reflns_number_total 8685 _reflns_number_gt 8345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2000)' _computing_publication_material 'SHELXTL (Sheldrick, 2000)' _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^)+(0.0225P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(4) _refine_ls_number_reflns 8685 _refine_ls_number_parameters 376 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0202 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0398 _refine_ls_wR_factor_gt 0.0394 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Lu1 Lu -0.247800(4) -0.185471(5) -0.250290(4) 0.01184(1) Uani 1 1 d . . . S1 S 0.20231(5) -0.36196(4) -0.15886(3) 0.01886(10) Uani 1 1 d . . . Si1 Si -0.35252(6) -0.31838(4) -0.45006(3) 0.01795(11) Uani 1 1 d . . . Si2 Si -0.35569(6) -0.42656(4) -0.11386(3) 0.01977(11) Uani 1 1 d D . . N1 N -0.01686(16) -0.28738(12) -0.23934(9) 0.0152(3) Uani 1 1 d . . . N2 N -0.10104(16) -0.12417(12) -0.13835(8) 0.0147(3) Uani 1 1 d . . . N3 N -0.31023(16) -0.01177(12) -0.21043(8) 0.0149(3) Uani 1 1 d . . . C1 C 0.2490(2) -0.52429(17) -0.28061(12) 0.0249(5) Uani 1 1 d . . . H1A H 0.2116 -0.5475 -0.3337 0.037 Uiso 1 1 calc R . . H1B H 0.2448 -0.5905 -0.2440 0.037 Uiso 1 1 calc R . . H1C H 0.3484 -0.4988 -0.2841 0.037 Uiso 1 1 calc R . . C2 C 0.16090(19) -0.42669(16) -0.25000(11) 0.0199(4) Uani 1 1 d . . . C3 C 0.04247(19) -0.37521(16) -0.28309(11) 0.0184(4) Uani 1 1 d . . . H3A H 0.0026 -0.3984 -0.3337 0.022 Uiso 1 1 calc R . . C4 C 0.05781(18) -0.27121(16) -0.17166(10) 0.0152(4) Uani 1 1 d . . . C5 C 0.01741(19) -0.18339(14) -0.11399(10) 0.0150(4) Uani 1 1 d . . . C6 C 0.0918(2) -0.15932(16) -0.04283(11) 0.0205(4) Uani 1 1 d . . . H6A H 0.1746 -0.2023 -0.0267 0.025 Uiso 1 1 calc R . . C7 C 0.0413(2) -0.07029(16) 0.00407(11) 0.0247(5) Uani 1 1 d . . . H7A H 0.0888 -0.0521 0.0537 0.030 Uiso 1 1 calc R . . C8 C -0.0777(2) -0.00815(17) -0.02133(11) 0.0250(5) Uani 1 1 d . . . H8A H -0.1115 0.0537 0.0103 0.030 Uiso 1 1 calc R . . C9 C -0.1489(2) -0.03638(15) -0.09396(10) 0.0177(4) Uani 1 1 d . . . C10 C -0.2855(2) 0.02334(16) -0.12556(11) 0.0202(4) Uani 1 1 d . . . C11 C -0.2696(3) 0.15551(17) -0.11262(13) 0.0338(6) Uani 1 1 d . . . H11A H -0.1857 0.1835 -0.1400 0.051 Uiso 1 1 calc R . . H11B H -0.2577 0.1719 -0.0553 0.051 Uiso 1 1 calc R . . H11C H -0.3553 0.1951 -0.1343 0.051 Uiso 1 1 calc R . . C12 C -0.4055(2) -0.0208(2) -0.07210(11) 0.0329(6) Uani 1 1 d . . . H12A H -0.4213 -0.1039 -0.0817 0.049 Uiso 1 1 calc R . . H12B H -0.4939 0.0219 -0.0850 0.049 Uiso 1 1 calc R . . H12C H -0.3771 -0.0084 -0.0158 0.049 Uiso 1 1 calc R . . C13 C -0.37501(19) 0.07599(14) -0.26119(10) 0.0141(4) Uani 1 1 d . . . C14 C -0.5249(2) 0.08185(15) -0.27430(10) 0.0182(4) Uani 1 1 d . . . C15 C -0.5848(2) 0.17273(16) -0.31994(12) 0.0221(4) Uani 1 1 d . . . H15A H -0.6856 0.1765 -0.3287 0.027 Uiso 1 1 calc R . . C16 C -0.4999(2) 0.25709(16) -0.35251(11) 0.0218(4) Uani 1 1 d . . . H16A H -0.5422 0.3204 -0.3811 0.026 Uiso 1 1 calc R . . C17 C -0.3529(2) 0.24854(15) -0.34314(11) 0.0191(4) Uani 1 1 d . . . H17A H -0.2947 0.3051 -0.3673 0.023 Uiso 1 1 calc R . . C18 C -0.2882(2) 0.15858(14) -0.29901(11) 0.0154(4) Uani 1 1 d . . . C19 C -0.6243(2) -0.01043(17) -0.24230(11) 0.0220(4) Uani 1 1 d . . . H19A H -0.5663 -0.0615 -0.2052 0.026 Uiso 1 1 calc R . . C20 C -0.7445(2) 0.0430(2) -0.19468(14) 0.0347(6) Uani 1 1 d . . . H20A H -0.7029 0.0907 -0.1512 0.052 Uiso 1 1 calc R . . H20B H -0.8022 -0.0191 -0.1723 0.052 Uiso 1 1 calc R . . H20C H -0.8052 0.0916 -0.2301 0.052 Uiso 1 1 calc R . . C21 C -0.6841(3) -0.08634(18) -0.31105(14) 0.0327(5) Uani 1 1 d . . . H21A H -0.6048 -0.1205 -0.3395 0.049 Uiso 1 1 calc R . . H21B H -0.7427 -0.0386 -0.3481 0.049 Uiso 1 1 calc R . . H21C H -0.7428 -0.1485 -0.2895 0.049 Uiso 1 1 calc R . . C22 C -0.1262(2) 0.14881(16) -0.29603(12) 0.0202(4) Uani 1 1 d . . . H22A H -0.0970 0.0954 -0.2511 0.024 Uiso 1 1 calc R . . C23 C -0.0493(2) 0.26577(19) -0.28208(14) 0.0326(5) Uani 1 1 d . . . H23A H -0.0798 0.3003 -0.2321 0.049 Uiso 1 1 calc R . . H23B H -0.0735 0.3184 -0.3266 0.049 Uiso 1 1 calc R . . H23C H 0.0542 0.2531 -0.2787 0.049 Uiso 1 1 calc R . . C24 C -0.0756(2) 0.09559(19) -0.37437(13) 0.0293(5) Uani 1 1 d . . . H24A H -0.1212 0.0198 -0.3830 0.044 Uiso 1 1 calc R . . H24B H 0.0285 0.0858 -0.3708 0.044 Uiso 1 1 calc R . . H24C H -0.1017 0.1473 -0.4191 0.044 Uiso 1 1 calc R . . C25 C -0.2679(2) -0.19914(15) -0.39191(11) 0.0185(4) Uani 1 1 d . . . H25A H -0.3175 -0.1274 -0.4102 0.022 Uiso 1 1 calc R . . H25B H -0.1691 -0.1933 -0.4105 0.022 Uiso 1 1 calc R . . C26 C -0.3494(2) -0.29829(16) -0.56174(11) 0.0240(5) Uani 1 1 d . . . H26A H -0.3993 -0.2263 -0.5769 0.036 Uiso 1 1 calc R . . H26B H -0.3971 -0.3642 -0.5885 0.036 Uiso 1 1 calc R . . H26C H -0.2501 -0.2940 -0.5779 0.036 Uiso 1 1 calc R . . C27 C -0.5451(2) -0.33866(18) -0.42622(12) 0.0288(5) Uani 1 1 d . . . H27A H -0.6019 -0.2745 -0.4492 0.043 Uiso 1 1 calc R . . H27B H -0.5539 -0.3397 -0.3681 0.043 Uiso 1 1 calc R . . H27C H -0.5799 -0.4124 -0.4489 0.043 Uiso 1 1 calc R . . C28 C -0.2608(3) -0.46065(16) -0.42765(12) 0.0318(5) Uani 1 1 d . . . H28A H -0.2632 -0.4769 -0.3703 0.048 Uiso 1 1 calc R . . H28B H -0.1613 -0.4563 -0.4434 0.048 Uiso 1 1 calc R . . H28C H -0.3101 -0.5229 -0.4576 0.048 Uiso 1 1 calc R . . C29 C -0.3976(2) -0.32686(16) -0.19761(12) 0.0201(4) Uani 1 1 d . A . H29A H -0.4848 -0.2848 -0.1828 0.024 Uiso 1 1 calc R . . H29B H -0.4268 -0.3773 -0.2433 0.024 Uiso 1 1 calc R . . C30 C -0.3166(7) -0.3479(4) -0.0170(2) 0.0434(15) Uani 0.506(7) 1 d PDU A 1 H30A H -0.2386 -0.2925 -0.0238 0.065 Uiso 0.506(7) 1 calc PR A 1 H30B H -0.2886 -0.4041 0.0247 0.065 Uiso 0.506(7) 1 calc PR A 1 H30C H -0.4023 -0.3060 -0.0015 0.065 Uiso 0.506(7) 1 calc PR A 1 C30' C -0.3832(8) -0.3516(4) -0.0163(2) 0.0459(17) Uani 0.494(7) 1 d PDU A 2 H30D H -0.3249 -0.2810 -0.0132 0.069 Uiso 0.494(7) 1 calc PR A 2 H30E H -0.3548 -0.4037 0.0278 0.069 Uiso 0.494(7) 1 calc PR A 2 H30F H -0.4842 -0.3311 -0.0126 0.069 Uiso 0.494(7) 1 calc PR A 2 C31 C -0.1800(2) -0.4987(2) -0.12638(18) 0.0536(7) Uani 1 1 d . A . H31A H -0.1028 -0.4445 -0.1113 0.080 Uiso 1 1 calc R . . H31B H -0.1717 -0.5218 -0.1823 0.080 Uiso 1 1 calc R . . H31C H -0.1730 -0.5676 -0.0921 0.080 Uiso 1 1 calc R . . C32 C -0.4844(2) -0.5512(2) -0.10557(17) 0.0462(7) Uani 1 1 d . A . H32A H -0.4875 -0.5958 -0.1555 0.069 Uiso 1 1 calc R . . H32B H -0.5800 -0.5209 -0.0958 0.069 Uiso 1 1 calc R . . H32C H -0.4528 -0.6017 -0.0612 0.069 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 Lu1 0.01293(2) 0.01083(2) 0.01159(2) 0.00027(5) -0.00144(2) 0.00067(5) S1 0.01423(19) 0.0202(2) 0.0218(2) 0.00033(19) -0.00308(17) 0.00229(17) Si1 0.0255(3) 0.0136(2) 0.0143(2) 0.00103(19) -0.0042(2) -0.0011(2) Si2 0.0220(2) 0.0188(2) 0.0186(2) 0.0067(2) 0.0021(2) 0.0023(2) N1 0.0150(7) 0.0145(7) 0.0160(7) 0.0001(6) -0.0007(6) -0.0003(6) N2 0.0175(7) 0.0117(6) 0.0146(6) 0.0012(6) -0.0024(6) -0.0032(6) N3 0.0223(7) 0.0114(6) 0.0108(6) 0.0026(5) -0.0029(6) 0.0034(6) C1 0.0197(9) 0.0242(9) 0.0309(9) -0.0044(8) 0.0005(9) 0.0054(8) C2 0.0166(8) 0.0216(9) 0.0216(8) -0.0020(8) 0.0019(7) -0.0020(7) C3 0.0151(8) 0.0233(9) 0.0168(8) -0.0023(7) 0.0009(7) 0.0004(7) C4 0.0105(7) 0.0156(7) 0.0195(8) 0.0025(7) -0.0014(7) -0.0014(7) C5 0.0168(8) 0.0131(7) 0.0149(8) 0.0014(7) -0.0021(7) -0.0042(7) C6 0.0236(9) 0.0172(8) 0.0201(9) 0.0015(7) -0.0085(8) -0.0028(7) C7 0.0373(11) 0.0187(9) 0.0170(8) -0.0024(7) -0.0127(8) -0.0032(8) C8 0.0418(11) 0.0159(9) 0.0167(8) -0.0033(7) -0.0052(8) 0.0016(8) C9 0.0255(9) 0.0127(8) 0.0148(8) 0.0008(7) -0.0001(7) -0.0014(7) C10 0.0283(10) 0.0164(8) 0.0158(8) 0.0003(7) -0.0012(7) 0.0081(7) C11 0.0575(14) 0.0212(9) 0.0215(10) -0.0073(8) -0.0128(10) 0.0142(10) C12 0.0338(11) 0.0497(13) 0.0155(9) 0.0001(9) 0.0039(8) 0.0100(10) C13 0.0189(8) 0.0106(7) 0.0126(7) 0.0000(6) -0.0006(6) 0.0025(6) C14 0.0194(8) 0.0163(8) 0.0192(8) 0.0025(7) 0.0031(7) 0.0028(7) C15 0.0177(9) 0.0223(9) 0.0265(9) 0.0041(8) 0.0015(8) 0.0070(7) C16 0.0270(10) 0.0163(8) 0.0219(9) 0.0045(7) -0.0011(8) 0.0078(8) C17 0.0278(9) 0.0105(8) 0.0190(8) 0.0029(7) 0.0017(8) -0.0007(7) C18 0.0187(8) 0.0117(7) 0.0156(8) -0.0028(6) -0.0010(7) -0.0003(6) C19 0.0174(9) 0.0229(9) 0.0260(9) 0.0057(8) 0.0046(7) 0.0019(7) C20 0.0238(10) 0.0399(12) 0.0413(11) 0.0096(10) 0.0127(9) 0.0023(9) C21 0.0350(11) 0.0274(11) 0.0358(11) 0.0037(9) 0.0020(9) -0.0101(9) C22 0.0169(8) 0.0157(8) 0.0276(9) 0.0030(7) -0.0038(8) -0.0027(7) C23 0.0287(11) 0.0243(10) 0.0439(12) -0.0004(10) -0.0091(10) -0.0093(9) C24 0.0193(9) 0.0313(11) 0.0377(11) -0.0047(9) 0.0036(9) -0.0023(8) C25 0.0251(9) 0.0144(8) 0.0156(8) 0.0012(7) -0.0033(7) 0.0000(7) C26 0.0313(10) 0.0240(10) 0.0164(8) -0.0010(7) -0.0017(8) 0.0012(8) C27 0.0308(11) 0.0345(11) 0.0206(9) 0.0019(8) -0.0031(9) -0.0075(9) C28 0.0503(13) 0.0150(9) 0.0289(10) 0.0006(8) -0.0144(10) 0.0006(9) C29 0.0163(8) 0.0202(9) 0.0235(9) 0.0054(7) -0.0014(7) 0.0003(7) C30 0.064(4) 0.043(3) 0.024(2) 0.012(2) 0.005(2) 0.003(2) C30' 0.070(4) 0.040(3) 0.029(2) 0.000(2) 0.014(2) -0.002(3) C31 0.0270(11) 0.0490(13) 0.0857(18) 0.0485(13) 0.0127(12) 0.0146(11) C32 0.0273(11) 0.0364(12) 0.0748(16) 0.0330(12) 0.0012(11) 0.0020(10) _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 Lu1 N3 2.1949(14) . ? Lu1 C29 2.3443(19) . ? Lu1 C25 2.3764(18) . ? Lu1 N2 2.3856(14) . ? Lu1 N1 2.4607(15) . ? S1 C4 1.7160(18) . ? S1 C2 1.7281(19) . ? Si1 C25 1.8433(18) . ? Si1 C27 1.877(2) . ? Si1 C28 1.880(2) . ? Si1 C26 1.8857(19) . ? Si2 C29 1.8422(19) . ? Si2 C31 1.862(2) . ? Si2 C30' 1.874(3) . ? Si2 C30 1.880(3) . ? Si2 C32 1.883(2) . ? N1 C4 1.320(2) . ? N1 C3 1.379(2) . ? N2 C9 1.342(2) . ? N2 C5 1.351(2) . ? N3 C13 1.439(2) . ? N3 C10 1.487(2) . ? C1 C2 1.497(3) . ? C2 C3 1.356(2) . ? C4 C5 1.459(2) . ? C5 C6 1.384(3) . ? C6 C7 1.386(3) . ? C7 C8 1.377(3) . ? C8 C9 1.401(3) . ? C9 C10 1.528(3) . ? C10 C11 1.543(3) . ? C10 C12 1.550(3) . ? C13 C14 1.414(3) . ? C13 C18 1.417(2) . ? C14 C15 1.399(3) . ? C14 C19 1.524(3) . ? C15 C16 1.381(3) . ? C16 C17 1.383(3) . ? C17 C18 1.396(2) . ? C18 C22 1.521(3) . ? C19 C21 1.533(3) . ? C19 C20 1.534(3) . ? C22 C24 1.540(3) . ? C22 C23 1.540(3) . ? 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 Lu1 C29 110.33(6) . . ? N3 Lu1 C25 110.64(6) . . ? C29 Lu1 C25 107.76(7) . . ? N3 Lu1 N2 69.12(5) . . ? C29 Lu1 N2 104.14(6) . . ? C25 Lu1 N2 145.43(6) . . ? N3 Lu1 N1 130.98(5) . . ? C29 Lu1 N1 100.28(6) . . ? C25 Lu1 N1 94.40(6) . . ? N2 Lu1 N1 66.79(5) . . ? C4 S1 C2 90.27(9) . . ? C25 Si1 C27 112.10(9) . . ? C25 Si1 C28 111.11(9) . . ? C27 Si1 C28 106.51(10) . . ? C25 Si1 C26 114.13(9) . . ? C27 Si1 C26 106.26(9) . . ? C28 Si1 C26 106.23(9) . . ? C29 Si2 C31 110.73(10) . . ? C29 Si2 C30' 110.13(17) . . ? C31 Si2 C30' 117.2(2) . . ? C29 Si2 C30 112.59(15) . . ? C31 Si2 C30 99.8(2) . . ? C30' Si2 C30 19.2(3) . . ? C29 Si2 C32 114.43(10) . . ? C31 Si2 C32 103.88(11) . . ? C30' Si2 C32 100.1(2) . . ? C30 Si2 C32 113.98(19) . . ? C4 N1 C3 110.41(15) . . ? C4 N1 Lu1 115.46(11) . . ? C3 N1 Lu1 133.00(11) . . ? C9 N2 C5 120.09(15) . . ? C9 N2 Lu1 117.58(11) . . ? C5 N2 Lu1 121.85(11) . . ? C13 N3 C10 114.79(13) . . ? C13 N3 Lu1 124.85(10) . . ? C10 N3 Lu1 120.36(10) . . ? C3 C2 C1 129.89(17) . . ? C3 C2 S1 108.84(14) . . ? C1 C2 S1 121.26(14) . . ? C2 C3 N1 116.36(16) . . ? N1 C4 C5 121.56(16) . . ? N1 C4 S1 114.13(13) . . ? C5 C4 S1 124.31(13) . . ? N2 C5 C6 122.52(16) . . ? N2 C5 C4 112.44(15) . . ? C6 C5 C4 125.02(16) . . ? C5 C6 C7 117.69(17) . . ? C8 C7 C6 119.97(17) . . ? C7 C8 C9 119.89(17) . . ? N2 C9 C8 119.81(17) . . ? N2 C9 C10 116.16(15) . . ? C8 C9 C10 123.96(16) . . ? N3 C10 C9 107.71(14) . . ? N3 C10 C11 114.37(15) . . ? C9 C10 C11 108.68(16) . . ? N3 C10 C12 112.00(16) . . ? C9 C10 C12 105.57(15) . . ? C11 C10 C12 108.09(17) . . ? C14 C13 C18 118.85(15) . . ? C14 C13 N3 121.17(15) . . ? C18 C13 N3 119.98(15) . . ? C15 C14 C13 119.60(17) . . ? C15 C14 C19 118.42(17) . . ? C13 C14 C19 121.94(15) . . ? C16 C15 C14 121.13(18) . . ? C15 C16 C17 119.43(17) . . ? C16 C17 C18 121.42(17) . . ? C17 C18 C13 119.35(17) . . ? C17 C18 C22 118.90(16) . . ? C13 C18 C22 121.69(15) . . ? C14 C19 C21 110.05(16) . . ? C14 C19 C20 112.00(17) . . ? C21 C19 C20 111.48(17) . . ? C18 C22 C24 110.03(15) . . ? C18 C22 C23 113.57(16) . . ? C24 C22 C23 108.61(17) . . ? Si1 C25 Lu1 126.26(9) . . ? Si2 C29 Lu1 127.36(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.338 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.052 _publ_section_references ; Data Collection, Reduction and Correction Program, CrysAlis Pro – Software Package, Agilent Technologies (2012) SCALE3 ABSPACK: Empirical absorption correction, CrysAlis Pro – Software Package, Agilent Technologies (2012) Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; _publ_contact_author 'Anton V. Cherkasov' _publ_contact_author_email 'ach@iomc.ras.ru' _publ_author_name 'L. Luconi, D. Lyubov, A. Rossin, A. Cherkasov, G. Tuci, G. Fukin, A. Trifonov, G. Giambastiani' _journal_name_full 'Organometallics' data_eramps _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H52 Er N3 S Si2' _chemical_formula_weight 734.27 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' 'S' 'S' 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M 'Pn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 9.38846(17) _cell_length_b 11.5607(3) _cell_length_c 16.7385(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.0783(17) _cell_angle_gamma 90.00 _cell_volume 1815.55(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21390 _cell_measurement_theta_min 3.0012 _cell_measurement_theta_max 32.4878 _exptl_crystal_description stick _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 754 _exptl_absorpt_coefficient_mu 2.458 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.4397 _exptl_absorpt_correction_T_max 0.7912 _exptl_absorpt_process_details ; SCALE3 ABSPACK, CrysAlisPro, Agilent Technologies (2012) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31012 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 28.00 _reflns_number_total 8753 _reflns_number_gt 8513 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2000)' _computing_publication_material 'SHELXTL (Sheldrick, 2000)' _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^)+(0.0237P)^2^+0.1963P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.023(4) _refine_ls_number_reflns 8753 _refine_ls_number_parameters 370 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0183 _refine_ls_R_factor_gt 0.0174 _refine_ls_wR_factor_ref 0.0402 _refine_ls_wR_factor_gt 0.0399 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.247892(4) 0.183862(4) 0.250390(4) 0.01214(1) Uani 1 1 d . . . S1 S -0.20270(4) 0.36152(4) 0.15741(3) 0.01888(9) Uani 1 1 d . . . Si1 Si 0.35309(5) 0.31975(4) 0.45064(3) 0.01831(10) Uani 1 1 d . . . Si2 Si 0.35580(5) 0.42595(4) 0.11255(3) 0.02060(10) Uani 1 1 d D . . N1 N 0.01400(14) 0.28638(12) 0.23847(8) 0.0168(3) Uani 1 1 d . . . N2 N 0.09835(14) 0.12219(11) 0.13721(8) 0.0149(3) Uani 1 1 d . . . N3 N 0.30821(14) 0.00965(11) 0.20786(8) 0.0150(3) Uani 1 1 d . . . C1 C -0.25021(19) 0.52428(15) 0.27878(11) 0.0244(4) Uani 1 1 d . . . H1A H -0.2151 0.5462 0.3325 0.037 Uiso 1 1 calc R . . H1B H -0.3501 0.5002 0.2807 0.037 Uiso 1 1 calc R . . H1C H -0.2427 0.5906 0.2427 0.037 Uiso 1 1 calc R . . C2 C -0.16256(17) 0.42609(14) 0.24875(10) 0.0196(4) Uani 1 1 d . . . C3 C -0.04539(18) 0.37441(14) 0.28230(10) 0.0192(4) Uani 1 1 d . . . H3A H -0.0063 0.3973 0.3330 0.023 Uiso 1 1 calc R . . C4 C -0.05951(16) 0.27101(14) 0.17048(9) 0.0154(3) Uani 1 1 d . . . C5 C -0.01926(18) 0.18218(13) 0.11320(10) 0.0160(3) Uani 1 1 d . . . C6 C -0.09342(19) 0.15943(15) 0.04167(10) 0.0215(4) Uani 1 1 d . . . H6A H -0.1751 0.2034 0.0257 0.026 Uiso 1 1 calc R . . C7 C -0.0445(2) 0.07055(15) -0.00574(10) 0.0248(4) Uani 1 1 d . . . H7A H -0.0924 0.0527 -0.0552 0.030 Uiso 1 1 calc R . . C8 C 0.0747(2) 0.00790(15) 0.01940(10) 0.0243(4) Uani 1 1 d . . . H8A H 0.1085 -0.0534 -0.0126 0.029 Uiso 1 1 calc R . . C9 C 0.14504(18) 0.03515(13) 0.09225(9) 0.0168(3) Uani 1 1 d . . . C10 C 0.28059(19) -0.02509(14) 0.12265(10) 0.0194(4) Uani 1 1 d . . . C11 C 0.2648(2) -0.15711(15) 0.10982(11) 0.0317(5) Uani 1 1 d . . . H11A H 0.1832 -0.1854 0.1391 0.048 Uiso 1 1 calc R . . H11B H 0.3517 -0.1962 0.1296 0.048 Uiso 1 1 calc R . . H11C H 0.2494 -0.1733 0.0527 0.048 Uiso 1 1 calc R . . C12 C 0.4008(2) 0.01774(19) 0.06851(11) 0.0324(5) Uani 1 1 d . . . H12A H 0.4180 0.1003 0.0781 0.049 Uiso 1 1 calc R . . H12B H 0.3719 0.0058 0.0123 0.049 Uiso 1 1 calc R . . H12C H 0.4884 -0.0258 0.0810 0.049 Uiso 1 1 calc R . . C13 C 0.37211(16) -0.07765(12) 0.25822(9) 0.0141(3) Uani 1 1 d . . . C14 C 0.52187(17) -0.08366(14) 0.27155(10) 0.0184(4) Uani 1 1 d . . . C15 C 0.58145(19) -0.17422(14) 0.31737(11) 0.0230(4) Uani 1 1 d . . . H15A H 0.6819 -0.1783 0.3259 0.028 Uiso 1 1 calc R . . C16 C 0.49543(19) -0.25821(14) 0.35047(10) 0.0220(4) Uani 1 1 d . . . H16A H 0.5370 -0.3214 0.3791 0.026 Uiso 1 1 calc R . . C17 C 0.34925(18) -0.24902(14) 0.34136(10) 0.0191(4) Uani 1 1 d . . . H17A H 0.2908 -0.3048 0.3659 0.023 Uiso 1 1 calc R . . C18 C 0.28474(18) -0.15935(13) 0.29679(10) 0.0158(3) Uani 1 1 d . . . C19 C 0.62106(18) 0.00819(15) 0.23892(11) 0.0226(4) Uani 1 1 d . . . H19A H 0.5632 0.0586 0.2016 0.027 Uiso 1 1 calc R . . C20 C 0.7411(2) -0.04523(19) 0.19135(12) 0.0337(5) Uani 1 1 d . . . H20A H 0.6998 -0.0926 0.1478 0.051 Uiso 1 1 calc R . . H20B H 0.8011 -0.0938 0.2268 0.051 Uiso 1 1 calc R . . H20C H 0.7990 0.0165 0.1690 0.051 Uiso 1 1 calc R . . C21 C 0.6798(2) 0.08415(17) 0.30685(13) 0.0327(5) Uani 1 1 d . . . H21A H 0.6006 0.1206 0.3340 0.049 Uiso 1 1 calc R . . H21B H 0.7412 0.1442 0.2852 0.049 Uiso 1 1 calc R . . H21C H 0.7354 0.0365 0.3451 0.049 Uiso 1 1 calc R . . C22 C 0.12314(18) -0.14943(15) 0.29461(11) 0.0203(4) Uani 1 1 d . . . H22A H 0.0941 -0.0976 0.2491 0.024 Uiso 1 1 calc R . . C23 C 0.0455(2) -0.26537(16) 0.28246(13) 0.0305(5) Uani 1 1 d . . . H23A H 0.0765 -0.3018 0.2332 0.046 Uiso 1 1 calc R . . H23B H -0.0575 -0.2519 0.2785 0.046 Uiso 1 1 calc R . . H23C H 0.0682 -0.3163 0.3280 0.046 Uiso 1 1 calc R . . C24 C 0.0736(2) -0.09351(17) 0.37186(12) 0.0301(5) Uani 1 1 d . . . H24A H 0.1207 -0.0185 0.3794 0.045 Uiso 1 1 calc R . . H24B H 0.0983 -0.1440 0.4173 0.045 Uiso 1 1 calc R . . H24C H -0.0299 -0.0823 0.3682 0.045 Uiso 1 1 calc R . . C25 C 0.26710(19) 0.20040(13) 0.39433(10) 0.0184(4) Uani 1 1 d . . . H25A H 0.1684 0.1962 0.4130 0.022 Uiso 1 1 calc R . . H25B H 0.3153 0.1289 0.4135 0.022 Uiso 1 1 calc R . . C26 C 0.3506(2) 0.30305(15) 0.56265(10) 0.0238(4) Uani 1 1 d . . . H26A H 0.4058 0.2345 0.5789 0.036 Uiso 1 1 calc R . . H26B H 0.2520 0.2942 0.5789 0.036 Uiso 1 1 calc R . . H26C H 0.3928 0.3718 0.5883 0.036 Uiso 1 1 calc R . . C27 C 0.5461(2) 0.33788(17) 0.42552(12) 0.0296(5) Uani 1 1 d . . . H27A H 0.6018 0.2732 0.4480 0.044 Uiso 1 1 calc R . . H27B H 0.5825 0.4107 0.4482 0.044 Uiso 1 1 calc R . . H27C H 0.5542 0.3391 0.3673 0.044 Uiso 1 1 calc R . . C28 C 0.2632(2) 0.46160(15) 0.42592(12) 0.0329(5) Uani 1 1 d . . . H28A H 0.1647 0.4595 0.4433 0.049 Uiso 1 1 calc R . . H28B H 0.2636 0.4746 0.3681 0.049 Uiso 1 1 calc R . . H28C H 0.3147 0.5245 0.4536 0.049 Uiso 1 1 calc R . . C29 C 0.39928(19) 0.32577(14) 0.19550(11) 0.0211(4) Uani 1 1 d . A . H29A H 0.4305 0.3754 0.2410 0.025 Uiso 1 1 calc R . . H29B H 0.4852 0.2833 0.1794 0.025 Uiso 1 1 calc R . . C30 C 0.3844(9) 0.3507(5) 0.0153(3) 0.0516(16) Uani 0.429(6) 1 d PD A 1 H30A H 0.3172 0.2861 0.0092 0.077 Uiso 0.429(6) 1 calc PR A 1 H30B H 0.4822 0.3212 0.0148 0.077 Uiso 0.429(6) 1 calc PR A 1 H30C H 0.3686 0.4054 -0.0288 0.077 Uiso 0.429(6) 1 calc PR A 1 C30' C 0.3133(7) 0.3484(4) 0.0151(2) 0.0516(16) Uani 0.571(6) 1 d PD A 2 H30D H 0.3986 0.3081 -0.0024 0.077 Uiso 0.571(6) 1 calc PR A 2 H30E H 0.2824 0.4048 -0.0257 0.077 Uiso 0.571(6) 1 calc PR A 2 H30F H 0.2370 0.2921 0.0228 0.077 Uiso 0.571(6) 1 calc PR A 2 C31 C 0.1826(2) 0.4996(2) 0.12834(17) 0.0572(7) Uani 1 1 d . A . H31A H 0.1041 0.4480 0.1119 0.086 Uiso 1 1 calc R . . H31B H 0.1773 0.5706 0.0964 0.086 Uiso 1 1 calc R . . H31C H 0.1754 0.5190 0.1851 0.086 Uiso 1 1 calc R . . C32 C 0.4847(2) 0.5491(2) 0.10204(16) 0.0502(6) Uani 1 1 d . A . H32A H 0.4898 0.5940 0.1517 0.075 Uiso 1 1 calc R . . H32B H 0.4521 0.5991 0.0578 0.075 Uiso 1 1 calc R . . H32C H 0.5793 0.5183 0.0911 0.075 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 Er1 0.01282(2) 0.01189(2) 0.01157(2) 0.00024(4) -0.00157(2) 0.00051(4) S1 0.01401(17) 0.02078(18) 0.02154(19) 0.00056(16) -0.00348(14) 0.00275(15) Si1 0.0258(2) 0.0143(2) 0.0145(2) 0.00106(16) -0.00431(18) -0.00170(17) Si2 0.0226(2) 0.0203(2) 0.0190(2) 0.00687(17) 0.00263(17) 0.00269(18) N1 0.0151(6) 0.0183(6) 0.0169(6) 0.0000(5) -0.0010(5) -0.0009(5) N2 0.0181(6) 0.0130(6) 0.0135(6) 0.0013(5) -0.0026(5) -0.0011(5) N3 0.0198(6) 0.0135(6) 0.0116(6) 0.0014(5) -0.0018(5) 0.0035(5) C1 0.0192(8) 0.0247(8) 0.0294(8) -0.0035(6) 0.0026(8) 0.0039(7) C2 0.0180(7) 0.0197(8) 0.0213(8) -0.0011(6) 0.0026(6) -0.0014(6) C3 0.0189(7) 0.0216(8) 0.0170(7) -0.0031(6) 0.0017(6) -0.0013(6) C4 0.0130(7) 0.0148(7) 0.0183(7) 0.0011(6) -0.0016(6) -0.0012(6) C5 0.0166(7) 0.0153(7) 0.0159(7) 0.0032(6) -0.0015(6) -0.0033(6) C6 0.0232(8) 0.0203(7) 0.0205(8) 0.0014(6) -0.0079(7) -0.0017(7) C7 0.0378(9) 0.0189(8) 0.0169(8) -0.0004(6) -0.0108(7) -0.0041(7) C8 0.0406(10) 0.0170(8) 0.0151(8) -0.0021(6) -0.0053(7) 0.0019(7) C9 0.0239(8) 0.0129(7) 0.0134(7) -0.0002(6) -0.0019(6) 0.0003(6) C10 0.0281(8) 0.0166(7) 0.0134(7) -0.0009(6) -0.0015(6) 0.0066(6) C11 0.0561(12) 0.0187(8) 0.0194(8) -0.0056(7) -0.0108(8) 0.0129(8) C12 0.0328(10) 0.0476(11) 0.0171(8) -0.0003(8) 0.0052(7) 0.0073(9) C13 0.0167(7) 0.0113(6) 0.0144(7) -0.0003(5) 0.0006(6) 0.0030(6) C14 0.0179(7) 0.0172(7) 0.0204(8) 0.0008(6) 0.0035(6) 0.0045(6) C15 0.0176(8) 0.0254(8) 0.0260(9) 0.0042(7) 0.0010(7) 0.0063(6) C16 0.0274(8) 0.0158(7) 0.0227(8) 0.0058(6) -0.0005(7) 0.0070(7) C17 0.0251(8) 0.0133(7) 0.0189(8) 0.0024(6) 0.0010(6) -0.0004(6) C18 0.0190(7) 0.0138(7) 0.0145(7) -0.0031(6) -0.0001(6) 0.0007(6) C19 0.0176(7) 0.0235(8) 0.0269(8) 0.0049(7) 0.0044(7) 0.0015(7) C20 0.0246(9) 0.0392(11) 0.0383(10) 0.0073(9) 0.0130(8) 0.0025(8) C21 0.0315(10) 0.0319(10) 0.0347(10) 0.0047(8) 0.0020(8) -0.0104(8) C22 0.0176(7) 0.0153(7) 0.0277(9) 0.0026(7) -0.0029(7) -0.0029(6) C23 0.0267(9) 0.0230(9) 0.0412(11) -0.0005(8) -0.0062(8) -0.0086(7) C24 0.0196(8) 0.0343(10) 0.0368(10) -0.0056(8) 0.0049(8) -0.0024(8) C25 0.0231(8) 0.0158(7) 0.0161(7) -0.0009(6) -0.0036(6) -0.0004(6) C26 0.0307(9) 0.0249(8) 0.0155(8) -0.0008(6) -0.0023(7) 0.0003(7) C27 0.0312(10) 0.0360(10) 0.0214(9) 0.0019(7) -0.0028(8) -0.0107(8) C28 0.0516(11) 0.0153(8) 0.0305(10) 0.0001(7) -0.0160(9) 0.0015(8) C29 0.0166(8) 0.0221(8) 0.0242(8) 0.0063(6) -0.0028(7) -0.0015(6) C30 0.091(5) 0.0436(14) 0.0201(12) 0.0050(11) 0.003(2) 0.003(2) C30' 0.091(5) 0.0436(14) 0.0201(12) 0.0050(11) 0.003(2) 0.003(2) C31 0.0302(11) 0.0514(12) 0.0911(17) 0.0483(12) 0.0162(11) 0.0171(10) C32 0.0239(10) 0.0425(11) 0.0838(16) 0.0422(11) -0.0006(10) 0.0006(9) _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 Er1 N3 2.2165(13) . ? Er1 C29 2.3771(17) . ? Er1 C25 2.4171(17) . ? Er1 N2 2.4239(13) . ? Er1 N1 2.4970(14) . ? S1 C4 1.7114(16) . ? S1 C2 1.7306(17) . ? Si1 C25 1.8408(17) . ? Si1 C28 1.8833(19) . ? Si1 C26 1.8859(18) . ? Si1 C27 1.886(2) . ? Si2 C29 1.8424(18) . ? Si2 C31 1.863(2) . ? Si2 C30 1.873(5) . ? Si2 C32 1.881(2) . ? Si2 C30' 1.892(4) . ? N1 C4 1.321(2) . ? N1 C3 1.384(2) . ? N2 C9 1.340(2) . ? N2 C5 1.353(2) . ? N3 C13 1.4326(19) . ? N3 C10 1.495(2) . ? C1 C2 1.499(2) . ? C2 C3 1.356(2) . ? C4 C5 1.464(2) . ? C5 C6 1.388(2) . ? C6 C7 1.387(2) . ? C7 C8 1.385(3) . ? C8 C9 1.402(2) . ? C9 C10 1.522(2) . ? C10 C11 1.548(2) . ? C10 C12 1.554(3) . ? C13 C14 1.417(2) . ? C13 C18 1.421(2) . ? C14 C15 1.402(2) . ? C14 C19 1.526(2) . ? C15 C16 1.391(2) . ? C16 C17 1.379(2) . ? C17 C18 1.402(2) . ? C18 C22 1.521(2) . ? C19 C21 1.524(3) . ? C19 C20 1.533(3) . ? C22 C24 1.533(3) . ? C22 C23 1.536(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 N3 Er1 C29 109.86(5) . . ? N3 Er1 C25 112.42(5) . . ? C29 Er1 C25 107.86(6) . . ? N3 Er1 N2 68.23(5) . . ? C29 Er1 N2 103.79(5) . . ? C25 Er1 N2 145.33(5) . . ? N3 Er1 N1 129.78(5) . . ? C29 Er1 N1 100.25(5) . . ? C25 Er1 N1 94.34(5) . . ? N2 Er1 N1 66.07(4) . . ? C4 S1 C2 90.34(8) . . ? C25 Si1 C28 110.83(8) . . ? C25 Si1 C26 114.29(8) . . ? C28 Si1 C26 106.62(9) . . ? C25 Si1 C27 112.09(9) . . ? C28 Si1 C27 106.29(9) . . ? C26 Si1 C27 106.23(9) . . ? C29 Si2 C31 110.56(10) . . ? C29 Si2 C30 109.1(2) . . ? C31 Si2 C30 119.3(3) . . ? C29 Si2 C32 114.87(9) . . ? C31 Si2 C32 103.60(10) . . ? C30 Si2 C32 99.1(2) . . ? C29 Si2 C30' 112.72(16) . . ? C31 Si2 C30' 100.4(2) . . ? C30 Si2 C30' 20.4(3) . . ? C32 Si2 C30' 113.22(19) . . ? C4 N1 C3 110.35(14) . . ? C4 N1 Er1 115.80(10) . . ? C3 N1 Er1 132.60(11) . . ? C9 N2 C5 119.89(14) . . ? C9 N2 Er1 117.90(10) . . ? C5 N2 Er1 121.66(10) . . ? C13 N3 C10 115.25(12) . . ? C13 N3 Er1 123.88(10) . . ? C10 N3 Er1 120.86(9) . . ? C3 C2 C1 129.92(16) . . ? C3 C2 S1 108.86(12) . . ? C1 C2 S1 121.21(12) . . ? C2 C3 N1 116.17(15) . . ? N1 C4 C5 121.29(14) . . ? N1 C4 S1 114.27(12) . . ? C5 C4 S1 124.44(12) . . ? N2 C5 C6 122.52(15) . . ? N2 C5 C4 113.11(14) . . ? C6 C5 C4 124.37(15) . . ? C7 C6 C5 117.89(16) . . ? C8 C7 C6 119.62(16) . . ? C7 C8 C9 119.79(16) . . ? N2 C9 C8 120.27(15) . . ? N2 C9 C10 116.26(13) . . ? C8 C9 C10 123.38(14) . . ? N3 C10 C9 108.06(13) . . ? N3 C10 C11 114.18(13) . . ? C9 C10 C11 109.26(14) . . ? N3 C10 C12 111.48(14) . . ? C9 C10 C12 106.00(13) . . ? C11 C10 C12 107.55(15) . . ? C14 C13 C18 118.78(14) . . ? C14 C13 N3 121.27(14) . . ? C18 C13 N3 119.95(14) . . ? C15 C14 C13 119.77(15) . . ? C15 C14 C19 118.60(15) . . ? C13 C14 C19 121.61(14) . . ? C16 C15 C14 120.88(16) . . ? C17 C16 C15 119.47(15) . . ? C16 C17 C18 121.64(15) . . ? C17 C18 C13 119.20(15) . . ? C17 C18 C22 118.68(15) . . ? C13 C18 C22 122.05(14) . . ? C21 C19 C14 110.05(15) . . ? C21 C19 C20 111.51(15) . . ? C14 C19 C20 112.03(15) . . ? C18 C22 C24 110.15(14) . . ? C18 C22 C23 113.93(14) . . ? C24 C22 C23 108.84(15) . . ? Si1 C25 Er1 125.81(8) . . ? Si2 C29 Er1 127.29(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.430 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.048 _publ_section_references ; Data Collection, Reduction and Correction Program, CrysAlis Pro - Software Package, Agilent Technologies (2012) SCALE3 ABSPACK: Empirical absorption correction, CrysAlis Pro - Software Package, Agilent Technologies (2012) Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; _publ_contact_author 'Anton V. Cherkasov' _publ_contact_author_email 'ach@iomc.ras.ru' _publ_author_name 'L. Luconi, D. Lyubov, A. Rossin, A. Cherkasov, G. Tuci, G. Fukin, A. Trifonov, G. Giambastiani' _journal_name_full 'Organometallics' data_ybampyrth _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H52 N3 S Si2 Yb' _chemical_formula_weight 740.05 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'Pn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 9.36372(12) _cell_length_b 11.54210(14) _cell_length_c 16.75309(18) _cell_angle_alpha 90.00 _cell_angle_beta 92.1653(11) _cell_angle_gamma 90.00 _cell_volume 1809.33(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16089 _cell_measurement_theta_min 3.5190 _cell_measurement_theta_max 31.2670 _exptl_crystal_description rhombus _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 758 _exptl_absorpt_coefficient_mu 2.732 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.4079 _exptl_absorpt_correction_T_max 0.8986 _exptl_absorpt_process_details ; SCALE3 ABSPACK, CrysAlisPro, Agilent Technologies (2012) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '/w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 29533 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7852 _reflns_number_gt 7466 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2000)' _computing_publication_material 'SHELXTL (Sheldrick, 2000)' _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^)+(0.0175P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.022(4) _refine_ls_number_reflns 7852 _refine_ls_number_parameters 365 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0214 _refine_ls_wR_factor_ref 0.0429 _refine_ls_wR_factor_gt 0.0421 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.752080(6) 0.816840(6) 0.749640(6) 0.01225(2) Uani 1 1 d . . . S1 S 1.20280(6) 0.63875(5) 0.84218(4) 0.01883(13) Uani 1 1 d . . . Si1 Si 0.64958(7) 0.68163(5) 0.55013(4) 0.01751(14) Uani 1 1 d . . . Si2 Si 0.64534(7) 0.57397(6) 0.88691(4) 0.02013(15) Uani 1 1 d U . . N1 N 0.98466(18) 0.71384(16) 0.76130(11) 0.0149(4) Uani 1 1 d . . . N2 N 0.89937(18) 0.87700(16) 0.86257(10) 0.0143(4) Uani 1 1 d . . . N3 N 0.69075(19) 0.98997(15) 0.79040(11) 0.0156(4) Uani 1 1 d . . . C1 C 1.2505(2) 0.4770(2) 0.72077(14) 0.0249(6) Uani 1 1 d . . . H1A H 1.2140 0.4536 0.6676 0.037 Uiso 1 1 calc R . . H1B H 1.2459 0.4111 0.7574 0.037 Uiso 1 1 calc R . . H1C H 1.3500 0.5026 0.7176 0.037 Uiso 1 1 calc R . . C2 C 1.1619(2) 0.5742(2) 0.75079(14) 0.0199(6) Uani 1 1 d . . . C3 C 1.0447(2) 0.6263(2) 0.71762(14) 0.0182(5) Uani 1 1 d . . . H3A H 1.0057 0.6038 0.6668 0.022 Uiso 1 1 calc R . . C4 C 1.0583(2) 0.7293(2) 0.82913(13) 0.0164(5) Uani 1 1 d . . . C5 C 1.0174(2) 0.8165(2) 0.88674(13) 0.0165(5) Uani 1 1 d . . . C6 C 1.0911(2) 0.8404(2) 0.95821(14) 0.0212(6) Uani 1 1 d . . . H6A H 1.1735 0.7971 0.9744 0.025 Uiso 1 1 calc R . . C7 C 1.0416(3) 0.9285(2) 1.00512(14) 0.0253(6) Uani 1 1 d . . . H7A H 1.0888 0.9455 1.0549 0.030 Uiso 1 1 calc R . . C8 C 0.9225(3) 0.9928(2) 0.97981(14) 0.0244(6) Uani 1 1 d . . . H8A H 0.8895 1.0552 1.0112 0.029 Uiso 1 1 calc R . . C9 C 0.8523(2) 0.96385(19) 0.90718(13) 0.0179(5) Uani 1 1 d . . . C10 C 0.7167(3) 1.0255(2) 0.87613(13) 0.0211(6) Uani 1 1 d . . . C11 C 0.7338(3) 1.1566(2) 0.88876(16) 0.0348(7) Uani 1 1 d . . . H11A H 0.8188 1.1836 0.8619 0.052 Uiso 1 1 calc R . . H11B H 0.7445 1.1731 0.9460 0.052 Uiso 1 1 calc R . . H11C H 0.6491 1.1966 0.8664 0.052 Uiso 1 1 calc R . . C12 C 0.5947(3) 0.9824(2) 0.92900(14) 0.0324(7) Uani 1 1 d . . . H12A H 0.5769 0.9000 0.9186 0.049 Uiso 1 1 calc R . . H12B H 0.5075 1.0267 0.9163 0.049 Uiso 1 1 calc R . . H12C H 0.6227 0.9933 0.9855 0.049 Uiso 1 1 calc R . . C13 C 0.6257(2) 1.07742(18) 0.74042(12) 0.0147(5) Uani 1 1 d . . . C14 C 0.4755(2) 1.08340(19) 0.72711(13) 0.0178(5) Uani 1 1 d . . . C15 C 0.4164(2) 1.1738(2) 0.68175(14) 0.0211(6) Uani 1 1 d . . . H15A H 0.3157 1.1777 0.6734 0.025 Uiso 1 1 calc R . . C16 C 0.5013(3) 1.2583(2) 0.64847(14) 0.0221(6) Uani 1 1 d . . . H16A H 0.4593 1.3212 0.6196 0.027 Uiso 1 1 calc R . . C17 C 0.6482(2) 1.24910(19) 0.65815(13) 0.0186(6) Uani 1 1 d . . . H17A H 0.7069 1.3053 0.6340 0.022 Uiso 1 1 calc R . . C18 C 0.7123(2) 1.15981(18) 0.70222(13) 0.0151(5) Uani 1 1 d . . . C19 C 0.3768(2) 0.9903(2) 0.75912(14) 0.0220(6) Uani 1 1 d . . . H19A H 0.4351 0.9397 0.7962 0.026 Uiso 1 1 calc R . . C20 C 0.2553(3) 1.0426(3) 0.80660(16) 0.0328(7) Uani 1 1 d . . . H20A H 0.2957 1.0939 0.8482 0.049 Uiso 1 1 calc R . . H20B H 0.2015 0.9802 0.8314 0.049 Uiso 1 1 calc R . . H20C H 0.1913 1.0870 0.7705 0.049 Uiso 1 1 calc R . . C21 C 0.3180(3) 0.9146(2) 0.69057(16) 0.0338(7) Uani 1 1 d . . . H21A H 0.3975 0.8796 0.6628 0.051 Uiso 1 1 calc R . . H21B H 0.2609 0.9624 0.6530 0.051 Uiso 1 1 calc R . . H21C H 0.2577 0.8535 0.7119 0.051 Uiso 1 1 calc R . . C22 C 0.8749(2) 1.1506(2) 0.70489(14) 0.0201(6) Uani 1 1 d . . . H22A H 0.9042 1.0977 0.7499 0.024 Uiso 1 1 calc R . . C23 C 0.9512(3) 1.2671(2) 0.71839(17) 0.0316(7) Uani 1 1 d . . . H23A H 0.9173 1.3034 0.7670 0.047 Uiso 1 1 calc R . . H23B H 0.9306 1.3180 0.6726 0.047 Uiso 1 1 calc R . . H23C H 1.0545 1.2541 0.7241 0.047 Uiso 1 1 calc R . . C24 C 0.9253(3) 1.0967(2) 0.62667(16) 0.0293(7) Uani 1 1 d . . . H24A H 0.8785 1.0215 0.6180 0.044 Uiso 1 1 calc R . . H24B H 1.0292 1.0858 0.6304 0.044 Uiso 1 1 calc R . . H24C H 0.9004 1.1484 0.5819 0.044 Uiso 1 1 calc R . . C25 C 0.7334(3) 0.80133(19) 0.60791(13) 0.0190(5) Uani 1 1 d . . . H25A H 0.6839 0.8726 0.5891 0.023 Uiso 1 1 calc R . . H25B H 0.8324 0.8070 0.5895 0.023 Uiso 1 1 calc R . . C26 C 0.6514(3) 0.7010(2) 0.43851(13) 0.0236(6) Uani 1 1 d . . . H26A H 0.6022 0.7732 0.4235 0.035 Uiso 1 1 calc R . . H26B H 0.6024 0.6356 0.4122 0.035 Uiso 1 1 calc R . . H26C H 0.7504 0.7044 0.4217 0.035 Uiso 1 1 calc R . . C27 C 0.4569(3) 0.6617(2) 0.57503(15) 0.0287(7) Uani 1 1 d . . . H27A H 0.3995 0.7243 0.5507 0.043 Uiso 1 1 calc R . . H27B H 0.4483 0.6636 0.6331 0.043 Uiso 1 1 calc R . . H27C H 0.4226 0.5870 0.5543 0.043 Uiso 1 1 calc R . . C28 C 0.7406(3) 0.5395(2) 0.57279(15) 0.0313(7) Uani 1 1 d . . . H28A H 0.8398 0.5431 0.5563 0.047 Uiso 1 1 calc R . . H28B H 0.6903 0.4772 0.5436 0.047 Uiso 1 1 calc R . . H28C H 0.7392 0.5242 0.6303 0.047 Uiso 1 1 calc R . . C29 C 0.6055(2) 0.6733(2) 0.80298(14) 0.0204(6) Uani 1 1 d . . . H29A H 0.5171 0.7143 0.8172 0.024 Uiso 1 1 calc R . . H29B H 0.5781 0.6226 0.7573 0.024 Uiso 1 1 calc R . . C30 C 0.6501(5) 0.6527(3) 0.98467(19) 0.0703(11) Uani 1 1 d U . . H30A H 0.7130 0.7202 0.9815 0.105 Uiso 1 1 calc R . . H30B H 0.6862 0.6007 1.0271 0.105 Uiso 1 1 calc R . . H30C H 0.5534 0.6783 0.9966 0.105 Uiso 1 1 calc R . . C31 C 0.8229(3) 0.5033(3) 0.8759(2) 0.0541(10) Uani 1 1 d . . . H31A H 0.8989 0.5566 0.8940 0.081 Uiso 1 1 calc R . . H31B H 0.8351 0.4835 0.8197 0.081 Uiso 1 1 calc R . . H31C H 0.8279 0.4326 0.9083 0.081 Uiso 1 1 calc R . . C32 C 0.5173(3) 0.4500(3) 0.8958(2) 0.0472(9) Uani 1 1 d . . . H32A H 0.5176 0.4032 0.8470 0.071 Uiso 1 1 calc R . . H32B H 0.4209 0.4802 0.9032 0.071 Uiso 1 1 calc R . . H32C H 0.5467 0.4019 0.9417 0.071 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 Yb1 0.01344(3) 0.01170(3) 0.01153(3) -0.00009(7) -0.00073(2) 0.00070(6) S1 0.0141(2) 0.0212(3) 0.0210(3) 0.0009(2) -0.0015(2) 0.0026(2) Si1 0.0251(3) 0.0135(3) 0.0136(3) 0.0019(3) -0.0033(2) -0.0012(3) Si2 0.0221(3) 0.0197(3) 0.0188(3) 0.0064(3) 0.0036(3) 0.0014(3) N1 0.0134(8) 0.0187(10) 0.0127(9) -0.0004(7) -0.0011(7) -0.0032(7) N2 0.0159(9) 0.0129(9) 0.0140(9) 0.0003(7) 0.0003(7) 0.0008(7) N3 0.0221(9) 0.0114(9) 0.0131(9) 0.0010(7) -0.0013(7) 0.0021(7) C1 0.0179(11) 0.0249(13) 0.0321(13) -0.0017(10) 0.0043(12) 0.0024(10) C2 0.0183(11) 0.0189(12) 0.0226(11) -0.0021(10) 0.0041(10) -0.0011(9) C3 0.0162(11) 0.0194(11) 0.0190(11) -0.0014(10) 0.0009(9) -0.0021(9) C4 0.0114(10) 0.0168(11) 0.0212(11) 0.0013(9) 0.0023(9) -0.0027(9) C5 0.0157(10) 0.0189(11) 0.0148(10) 0.0032(9) -0.0001(8) -0.0040(9) C6 0.0206(11) 0.0214(12) 0.0211(12) 0.0019(10) -0.0067(10) 0.0005(9) C7 0.0367(13) 0.0185(12) 0.0200(12) -0.0014(10) -0.0103(10) -0.0038(11) C8 0.0409(14) 0.0153(12) 0.0168(11) -0.0018(10) -0.0031(11) 0.0041(11) C9 0.0265(11) 0.0140(11) 0.0132(10) 0.0037(9) 0.0007(9) -0.0005(9) C10 0.0314(12) 0.0195(12) 0.0123(10) -0.0030(9) -0.0014(10) 0.0074(10) C11 0.0548(17) 0.0270(14) 0.0213(13) -0.0075(11) -0.0127(12) 0.0141(12) C12 0.0364(14) 0.0444(17) 0.0167(12) -0.0021(12) 0.0065(11) 0.0104(12) C13 0.0221(11) 0.0110(10) 0.0111(10) 0.0005(9) 0.0033(9) 0.0033(9) C14 0.0203(11) 0.0175(11) 0.0160(11) 0.0015(9) 0.0060(9) 0.0027(9) C15 0.0156(10) 0.0243(13) 0.0234(12) 0.0024(10) 0.0005(9) 0.0065(9) C16 0.0289(12) 0.0165(12) 0.0209(12) 0.0029(10) 0.0002(10) 0.0086(10) C17 0.0238(11) 0.0139(11) 0.0184(11) 0.0028(9) 0.0025(10) -0.0016(9) C18 0.0176(10) 0.0129(11) 0.0147(10) -0.0030(8) 0.0018(9) -0.0012(8) C19 0.0183(11) 0.0225(12) 0.0256(12) 0.0055(10) 0.0053(10) 0.0005(9) C20 0.0223(12) 0.0388(16) 0.0385(14) 0.0094(13) 0.0148(11) 0.0031(11) C21 0.0375(14) 0.0315(15) 0.0326(14) 0.0047(12) 0.0047(12) -0.0096(12) C22 0.0157(11) 0.0194(12) 0.0249(12) 0.0001(10) -0.0023(10) -0.0011(9) C23 0.0258(13) 0.0255(13) 0.0429(16) -0.0001(12) -0.0066(12) -0.0096(11) C24 0.0190(12) 0.0319(14) 0.0374(15) -0.0038(12) 0.0060(11) -0.0033(11) C25 0.0246(11) 0.0146(11) 0.0175(11) 0.0005(9) -0.0042(9) 0.0026(9) C26 0.0289(12) 0.0258(13) 0.0159(11) 0.0005(10) -0.0025(10) 0.0012(10) C27 0.0319(13) 0.0351(15) 0.0189(12) 0.0024(11) -0.0024(11) -0.0107(11) C28 0.0483(15) 0.0168(12) 0.0277(13) -0.0003(11) -0.0129(12) 0.0040(12) C29 0.0143(10) 0.0234(13) 0.0234(12) 0.0033(10) -0.0003(9) 0.0010(9) C30 0.132(3) 0.0519(19) 0.0269(14) 0.0033(14) 0.0085(18) 0.0014(19) C31 0.0269(14) 0.0458(17) 0.090(2) 0.0440(17) 0.0092(16) 0.0107(13) C32 0.0287(14) 0.0408(16) 0.072(2) 0.0339(16) 0.0009(14) -0.0007(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 Yb1 N3 2.1952(18) . ? Yb1 C29 2.349(2) . ? Yb1 C25 2.381(2) . ? Yb1 N2 2.4014(17) . ? Yb1 N1 2.4823(18) . ? S1 C4 1.717(2) . ? S1 C2 1.733(2) . ? Si1 C25 1.845(2) . ? Si1 C27 1.881(3) . ? Si1 C28 1.881(2) . ? Si1 C26 1.884(2) . ? Si2 C29 1.842(2) . ? Si2 C31 1.868(3) . ? Si2 C30 1.872(3) . ? Si2 C32 1.876(3) . ? N1 C4 1.319(3) . ? N1 C3 1.380(3) . ? N2 C9 1.335(3) . ? N2 C5 1.356(3) . ? N3 C13 1.433(3) . ? N3 C10 1.505(3) . ? C1 C2 1.494(3) . ? C2 C3 1.352(3) . ? C4 C5 1.456(3) . ? C5 C6 1.387(3) . ? C6 C7 1.377(3) . ? C7 C8 1.392(3) . ? C8 C9 1.401(3) . ? C9 C10 1.529(3) . ? C10 C11 1.535(3) . ? C10 C12 1.553(3) . ? C13 C14 1.417(3) . ? C13 C18 1.418(3) . ? C14 C15 1.393(3) . ? C14 C19 1.528(3) . ? C15 C16 1.388(3) . ? C16 C17 1.383(3) . ? C17 C18 1.391(3) . ? C18 C22 1.526(3) . ? C19 C21 1.529(4) . ? C19 C20 1.536(3) . ? C22 C23 1.535(3) . ? C22 C24 1.541(3) . ? 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 Yb1 C29 111.10(8) . . ? N3 Yb1 C25 111.62(7) . . ? C29 Yb1 C25 107.71(8) . . ? N3 Yb1 N2 68.96(6) . . ? C29 Yb1 N2 103.33(7) . . ? C25 Yb1 N2 145.67(7) . . ? N3 Yb1 N1 130.58(6) . . ? C29 Yb1 N1 98.97(7) . . ? C25 Yb1 N1 94.23(7) . . ? N2 Yb1 N1 66.45(6) . . ? C4 S1 C2 90.15(11) . . ? C25 Si1 C27 111.56(11) . . ? C25 Si1 C28 111.50(11) . . ? C27 Si1 C28 106.26(12) . . ? C25 Si1 C26 114.34(11) . . ? C27 Si1 C26 106.22(11) . . ? C28 Si1 C26 106.44(11) . . ? C29 Si2 C31 110.63(13) . . ? C29 Si2 C30 111.30(14) . . ? C31 Si2 C30 107.86(18) . . ? C29 Si2 C32 115.07(12) . . ? C31 Si2 C32 104.38(13) . . ? C30 Si2 C32 107.15(17) . . ? C4 N1 C3 110.22(18) . . ? C4 N1 Yb1 115.58(14) . . ? C3 N1 Yb1 133.07(14) . . ? C9 N2 C5 120.13(18) . . ? C9 N2 Yb1 117.79(14) . . ? C5 N2 Yb1 121.58(14) . . ? C13 N3 C10 114.56(17) . . ? C13 N3 Yb1 124.75(13) . . ? C10 N3 Yb1 120.68(13) . . ? C3 C2 C1 130.4(2) . . ? C3 C2 S1 108.70(17) . . ? C1 C2 S1 120.89(16) . . ? C2 C3 N1 116.6(2) . . ? N1 C4 C5 121.5(2) . . ? N1 C4 S1 114.28(17) . . ? C5 C4 S1 124.22(16) . . ? N2 C5 C6 121.9(2) . . ? N2 C5 C4 112.95(18) . . ? C6 C5 C4 125.1(2) . . ? C7 C6 C5 118.2(2) . . ? C6 C7 C8 120.2(2) . . ? C7 C8 C9 118.8(2) . . ? N2 C9 C8 120.7(2) . . ? N2 C9 C10 116.51(18) . . ? C8 C9 C10 122.7(2) . . ? N3 C10 C9 107.46(18) . . ? N3 C10 C11 114.35(19) . . ? C9 C10 C11 109.3(2) . . ? N3 C10 C12 111.17(19) . . ? C9 C10 C12 106.02(19) . . ? C11 C10 C12 108.2(2) . . ? C14 C13 C18 118.51(19) . . ? C14 C13 N3 121.59(19) . . ? C18 C13 N3 119.89(19) . . ? C15 C14 C13 119.6(2) . . ? C15 C14 C19 119.0(2) . . ? C13 C14 C19 121.37(19) . . ? C16 C15 C14 121.6(2) . . ? C17 C16 C15 118.8(2) . . ? C16 C17 C18 121.7(2) . . ? C17 C18 C13 119.6(2) . . ? C17 C18 C22 118.5(2) . . ? C13 C18 C22 121.83(19) . . ? C14 C19 C21 110.1(2) . . ? C14 C19 C20 112.1(2) . . ? C21 C19 C20 111.1(2) . . ? C18 C22 C23 113.70(19) . . ? C18 C22 C24 109.93(18) . . ? C23 C22 C24 108.9(2) . . ? Si1 C25 Yb1 126.39(11) . . ? Si2 C29 Yb1 128.68(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.495 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.066 _publ_section_references ; Data Collection, Reduction and Correction Program, CrysAlis Pro - Software Package, Agilent Technologies (2012) SCALE3 ABSPACK: Empirical absorption correction, CrysAlis Pro - Software Package, Agilent Technologies (2012) Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ;