# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_complex7 _database_code_depnum_ccdc_archive 'CCDC 915741' #TrackingRef '915741.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H81 N4 O2 Si2 Yb' _chemical_formula_sum 'C53 H81 N4 O2 Si2 Yb' _chemical_formula_weight 1035.44 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' Yb Yb -0.3850 5.5486 '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 'P 212121' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 13.244(4) _cell_length_b 19.003(6) _cell_length_c 21.832(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5495(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 19835 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2164 _exptl_absorpt_coefficient_mu 1.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.148 _exptl_absorpt_correction_T_max 0.247 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19391 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_unetI/netI 0.1010 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9737 _reflns_number_gt 8340 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their C50-C51',C50- C52', C50-C53',C50-C51,C50-C52,C50-C53,C6-C7,C8-C9,C9-C10, C6-C11 and N3-H3 distances were constrained. ; _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^)+(0.0791P)^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 -0.002(16) _refine_ls_number_reflns 9737 _refine_ls_number_parameters 572 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1670 _refine_ls_wR_factor_gt 0.1428 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.098 _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 Yb1 Yb 0.60914(3) 0.60714(2) 0.295773(19) 0.03442(14) Uani 1 1 d . . . Si1 Si 0.5224(2) 0.57741(19) 0.12509(14) 0.0464(8) Uani 1 1 d . . . Si2 Si 0.9593(2) 0.6699(2) 0.40404(15) 0.0479(8) Uani 1 1 d . . . O1 O 0.5345(5) 0.5464(4) 0.3599(3) 0.0375(16) Uani 1 1 d . . . O2 O 0.7556(5) 0.5934(4) 0.2651(3) 0.0417(18) Uani 1 1 d . . . N1 N 0.5282(6) 0.6148(4) 0.1968(4) 0.0368(17) Uani 1 1 d . . . N2 N 0.5045(7) 0.6967(5) 0.2713(4) 0.043(2) Uani 1 1 d . . . N3 N 0.8328(7) 0.6673(5) 0.3773(4) 0.045(2) Uani 1 1 d D . . H3 H 0.828(9) 0.630(3) 0.356(4) 0.054 Uiso 1 1 d D . . N4 N 0.6621(6) 0.6943(4) 0.3697(4) 0.0370(19) Uani 1 1 d . . . C1 C 0.4840(6) 0.6763(5) 0.2135(5) 0.036(2) Uani 1 1 d . . . C2 C 0.7503(9) 0.7105(7) 0.3941(5) 0.046(3) Uani 1 1 d . . . C3 C 0.4662(9) 0.7623(6) 0.2964(6) 0.052(3) Uani 1 1 d . . . H3A H 0.4005 0.7544 0.3159 0.062 Uiso 1 1 calc R . . H3B H 0.4573 0.7969 0.2635 0.062 Uiso 1 1 calc R . . C4 C 0.5430(9) 0.7905(7) 0.3445(5) 0.055(3) Uani 1 1 d . . . H4A H 0.6028 0.8079 0.3228 0.066 Uiso 1 1 calc R . . H4B H 0.5125 0.8307 0.3658 0.066 Uiso 1 1 calc R . . C5 C 0.5751(8) 0.7399(6) 0.3896(5) 0.041(2) Uani 1 1 d . . . H5A H 0.5177 0.7096 0.3998 0.049 Uiso 1 1 calc R . . H5B H 0.5945 0.7651 0.4270 0.049 Uiso 1 1 calc R . . C6 C 0.4151(7) 0.7185(6) 0.1744(4) 0.040(3) Uani 1 1 d D . . C7 C 0.4493(9) 0.7630(5) 0.1304(6) 0.052(3) Uani 1 1 d D . . H7 H 0.5194 0.7687 0.1255 0.062 Uiso 1 1 calc R . . C8 C 0.3855(11) 0.8000(6) 0.0929(6) 0.064(4) Uani 1 1 d D . . H8 H 0.4117 0.8315 0.0637 0.076 Uiso 1 1 calc R . . C9 C 0.2830(10) 0.7905(6) 0.0982(6) 0.058(3) Uani 1 1 d D . . H9 H 0.2390 0.8147 0.0719 0.069 Uiso 1 1 calc R . . C10 C 0.2443(8) 0.7458(6) 0.1419(5) 0.048(3) Uani 1 1 d D . . H10 H 0.1743 0.7398 0.1465 0.058 Uiso 1 1 calc R . . C11 C 0.3122(7) 0.7096(6) 0.1791(5) 0.041(3) Uani 1 1 d D . . H11 H 0.2868 0.6780 0.2084 0.049 Uiso 1 1 calc R . . C12 C 0.7648(9) 0.7635(7) 0.4398(5) 0.051(3) Uani 1 1 d . . . C13 C 0.7747(9) 0.7518(7) 0.5013(5) 0.046(3) Uani 1 1 d . . . H13 H 0.7716 0.7055 0.5164 0.055 Uiso 1 1 calc R . . C14 C 0.7894(10) 0.8080(10) 0.5424(6) 0.073(5) Uani 1 1 d . . . H14 H 0.7902 0.7987 0.5847 0.088 Uiso 1 1 calc R . . C15 C 0.8019(9) 0.8718(7) 0.5240(7) 0.064(4) Uani 1 1 d . . . H15 H 0.8200 0.9075 0.5517 0.077 Uiso 1 1 calc R . . C16 C 0.7879(10) 0.8866(8) 0.4615(7) 0.068(4) Uani 1 1 d . . . H16 H 0.7865 0.9333 0.4473 0.082 Uiso 1 1 calc R . . C17 C 0.7758(10) 0.8290(8) 0.4203(6) 0.062(3) Uani 1 1 d . . . H17 H 0.7757 0.8378 0.3779 0.075 Uiso 1 1 calc R . . C18 C 0.5870(16) 0.6259(8) 0.0635(6) 0.097(6) Uani 1 1 d . . . H18A H 0.5549 0.6713 0.0579 0.145 Uiso 1 1 calc R . . H18B H 0.5828 0.5992 0.0257 0.145 Uiso 1 1 calc R . . H18C H 0.6573 0.6327 0.0744 0.145 Uiso 1 1 calc R . . C19 C 0.3916(10) 0.5564(6) 0.0986(5) 0.055(3) Uani 1 1 d . . . H19A H 0.3830 0.5058 0.0969 0.083 Uiso 1 1 calc R . . H19B H 0.3810 0.5763 0.0582 0.083 Uiso 1 1 calc R . . H19C H 0.3431 0.5763 0.1270 0.083 Uiso 1 1 calc R . . C20 C 0.5963(11) 0.4974(8) 0.1305(6) 0.071(4) Uani 1 1 d . . . H20A H 0.6632 0.5085 0.1457 0.107 Uiso 1 1 calc R . . H20B H 0.6018 0.4761 0.0903 0.107 Uiso 1 1 calc R . . H20C H 0.5635 0.4649 0.1583 0.107 Uiso 1 1 calc R . . C21 C 1.0093(10) 0.7632(7) 0.4095(7) 0.069(4) Uani 1 1 d . . . H21A H 0.9893 0.7894 0.3734 0.103 Uiso 1 1 calc R . . H21B H 1.0824 0.7622 0.4123 0.103 Uiso 1 1 calc R . . H21C H 0.9818 0.7857 0.4457 0.103 Uiso 1 1 calc R . . C22 C 1.0312(9) 0.6217(9) 0.3450(7) 0.082(5) Uani 1 1 d . . . H22A H 1.0121 0.5724 0.3457 0.122 Uiso 1 1 calc R . . H22B H 1.1029 0.6260 0.3533 0.122 Uiso 1 1 calc R . . H22C H 1.0163 0.6414 0.3050 0.122 Uiso 1 1 calc R . . C23 C 0.9693(11) 0.6275(8) 0.4805(6) 0.073(4) Uani 1 1 d . . . H23A H 0.9416 0.6587 0.5114 0.109 Uiso 1 1 calc R . . H23B H 1.0396 0.6180 0.4896 0.109 Uiso 1 1 calc R . . H23C H 0.9317 0.5836 0.4803 0.109 Uiso 1 1 calc R . . C24 C 0.4866(7) 0.4965(5) 0.3962(5) 0.035(2) Uani 1 1 d . . . C25 C 0.3958(9) 0.4639(6) 0.3747(4) 0.047(3) Uani 1 1 d . . . C26 C 0.3510(9) 0.4164(5) 0.4121(5) 0.039(2) Uani 1 1 d . . . H26 H 0.2904 0.3957 0.3987 0.047 Uiso 1 1 calc R . . C27 C 0.3878(9) 0.3966(7) 0.4677(4) 0.054(3) Uani 1 1 d . . . C28 C 0.4720(8) 0.4288(5) 0.4886(5) 0.036(2) Uani 1 1 d . . . H28 H 0.4962 0.4166 0.5276 0.043 Uiso 1 1 calc R . . C29 C 0.5255(7) 0.4803(6) 0.4545(4) 0.036(2) Uani 1 1 d . . . C30 C 0.3505(9) 0.4824(7) 0.3116(5) 0.057(3) Uani 1 1 d . . . C31 C 0.4223(13) 0.4582(6) 0.2615(6) 0.074(5) Uani 1 1 d . . . H31A H 0.4885 0.4785 0.2684 0.110 Uiso 1 1 calc R . . H31B H 0.3969 0.4734 0.2220 0.110 Uiso 1 1 calc R . . H31C H 0.4272 0.4073 0.2621 0.110 Uiso 1 1 calc R . . C32 C 0.3246(9) 0.5611(6) 0.3062(6) 0.056(3) Uani 1 1 d . . . H32A H 0.2823 0.5750 0.3404 0.084 Uiso 1 1 calc R . . H32B H 0.2889 0.5695 0.2681 0.084 Uiso 1 1 calc R . . H32C H 0.3864 0.5885 0.3067 0.084 Uiso 1 1 calc R . . C33 C 0.2507(11) 0.4415(7) 0.3004(8) 0.081(5) Uani 1 1 d . . . H33A H 0.2641 0.3914 0.3012 0.122 Uiso 1 1 calc R . . H33B H 0.2232 0.4545 0.2608 0.122 Uiso 1 1 calc R . . H33C H 0.2024 0.4532 0.3322 0.122 Uiso 1 1 calc R . . C34 C 0.3379(10) 0.3378(7) 0.5036(5) 0.060(3) Uani 1 1 d . . . H34A H 0.3814 0.3239 0.5372 0.090 Uiso 1 1 calc R . . H34B H 0.3265 0.2979 0.4768 0.090 Uiso 1 1 calc R . . H34C H 0.2738 0.3542 0.5197 0.090 Uiso 1 1 calc R . . C35 C 0.6173(9) 0.5173(7) 0.4843(5) 0.048(3) Uani 1 1 d . . . C36 C 0.6481(11) 0.4823(9) 0.5440(6) 0.081(5) Uani 1 1 d . . . H36A H 0.5948 0.4882 0.5740 0.122 Uiso 1 1 calc R . . H36B H 0.7096 0.5038 0.5592 0.122 Uiso 1 1 calc R . . H36C H 0.6597 0.4325 0.5370 0.122 Uiso 1 1 calc R . . C37 C 0.7100(8) 0.5122(9) 0.4424(6) 0.071(4) Uani 1 1 d . . . H37A H 0.7683 0.5320 0.4632 0.107 Uiso 1 1 calc R . . H37B H 0.6974 0.5383 0.4050 0.107 Uiso 1 1 calc R . . H37C H 0.7230 0.4633 0.4326 0.107 Uiso 1 1 calc R . . C38 C 0.5868(11) 0.5936(7) 0.4985(6) 0.068(4) Uani 1 1 d . . . H38A H 0.5346 0.5939 0.5298 0.102 Uiso 1 1 calc R . . H38B H 0.5612 0.6158 0.4616 0.102 Uiso 1 1 calc R . . H38C H 0.6452 0.6194 0.5132 0.102 Uiso 1 1 calc R . . C39 C 0.8394(8) 0.5798(6) 0.2310(4) 0.039(2) Uani 1 1 d . . . C40 C 0.8809(9) 0.5109(6) 0.2332(4) 0.044(2) Uani 1 1 d . . . C41 C 0.9749(7) 0.4981(6) 0.2062(5) 0.043(2) Uani 1 1 d . . . H41 H 1.0023 0.4525 0.2077 0.052 Uiso 1 1 calc R . . C42 C 1.0284(8) 0.5512(6) 0.1774(5) 0.040(2) Uani 1 1 d . . . C43 C 0.9840(7) 0.6167(7) 0.1729(4) 0.043(3) Uani 1 1 d . . . H43 H 1.0181 0.6523 0.1514 0.051 Uiso 1 1 calc R . . C44 C 0.8902(7) 0.6320(5) 0.1990(4) 0.036(2) Uani 1 1 d . A . C45 C 0.8315(9) 0.4478(6) 0.2650(5) 0.048(3) Uani 1 1 d . . . C46 C 0.8429(12) 0.3805(6) 0.2193(7) 0.084(5) Uani 1 1 d . . . H46A H 0.8112 0.3911 0.1803 0.126 Uiso 1 1 calc R . . H46B H 0.8104 0.3398 0.2375 0.126 Uiso 1 1 calc R . . H46C H 0.9139 0.3704 0.2128 0.126 Uiso 1 1 calc R . . C47 C 0.7187(9) 0.4457(8) 0.2802(6) 0.065(4) Uani 1 1 d . . . H47A H 0.7019 0.4852 0.3065 0.097 Uiso 1 1 calc R . . H47B H 0.7031 0.4021 0.3012 0.097 Uiso 1 1 calc R . . H47C H 0.6798 0.4486 0.2427 0.097 Uiso 1 1 calc R . . C48 C 0.8896(12) 0.4340(9) 0.3265(6) 0.082(5) Uani 1 1 d . . . H48A H 0.9567 0.4542 0.3239 0.123 Uiso 1 1 calc R . . H48B H 0.8949 0.3837 0.3333 0.123 Uiso 1 1 calc R . . H48C H 0.8531 0.4555 0.3601 0.123 Uiso 1 1 calc R . . C49 C 1.1317(8) 0.5361(6) 0.1501(5) 0.047(3) Uani 1 1 d . . . H49A H 1.1298 0.5444 0.1063 0.071 Uiso 1 1 calc R . . H49B H 1.1497 0.4874 0.1578 0.071 Uiso 1 1 calc R . . H49C H 1.1814 0.5668 0.1687 0.071 Uiso 1 1 calc R . . C50 C 0.8493(7) 0.7060(6) 0.1913(5) 0.051(3) Uani 1 1 d D . . C51 C 0.858(2) 0.7299(13) 0.1235(8) 0.058(3) Uiso 0.50 1 d PD A 1 H51A H 0.8049 0.7080 0.0996 0.086 Uiso 0.50 1 calc PR A 1 H51B H 0.9233 0.7159 0.1073 0.086 Uiso 0.50 1 calc PR A 1 H51C H 0.8516 0.7807 0.1212 0.086 Uiso 0.50 1 calc PR A 1 C51' C 0.9198(18) 0.7555(12) 0.1534(11) 0.058(3) Uiso 0.50 1 d PD A 2 H51D H 0.9709 0.7755 0.1801 0.086 Uiso 0.50 1 calc PR A 2 H51E H 0.8801 0.7931 0.1354 0.086 Uiso 0.50 1 calc PR A 2 H51F H 0.9522 0.7287 0.1211 0.086 Uiso 0.50 1 calc PR A 2 C52 C 0.9169(19) 0.7591(12) 0.2234(11) 0.058(3) Uiso 0.50 1 d PD A 1 H52A H 0.9071 0.7557 0.2674 0.086 Uiso 0.50 1 calc PR A 1 H52B H 0.8998 0.8062 0.2098 0.086 Uiso 0.50 1 calc PR A 1 H52C H 0.9869 0.7492 0.2136 0.086 Uiso 0.50 1 calc PR A 1 C52' C 0.862(2) 0.7573(12) 0.2448(10) 0.058(3) Uiso 0.50 1 d PD A 2 H52D H 0.8248 0.7401 0.2800 0.086 Uiso 0.50 1 calc PR A 2 H52E H 0.8364 0.8032 0.2331 0.086 Uiso 0.50 1 calc PR A 2 H52F H 0.9331 0.7612 0.2552 0.086 Uiso 0.50 1 calc PR A 2 C53 C 0.7450(15) 0.7201(17) 0.2198(12) 0.058(3) Uiso 0.50 1 d PD A 1 H53A H 0.7228 0.6787 0.2421 0.086 Uiso 0.50 1 calc PR A 1 H53B H 0.6969 0.7308 0.1876 0.086 Uiso 0.50 1 calc PR A 1 H53C H 0.7495 0.7597 0.2477 0.086 Uiso 0.50 1 calc PR A 1 C53' C 0.7354(13) 0.7143(16) 0.1959(13) 0.058(3) Uiso 0.50 1 d PD A 2 H53D H 0.7084 0.6784 0.2229 0.086 Uiso 0.50 1 calc PR A 2 H53E H 0.7057 0.7092 0.1555 0.086 Uiso 0.50 1 calc PR A 2 H53F H 0.7194 0.7604 0.2122 0.086 Uiso 0.50 1 calc PR A 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 Yb1 0.0284(2) 0.0374(2) 0.0375(2) -0.0012(2) 0.00597(19) -0.0005(2) Si1 0.0302(15) 0.068(2) 0.0413(17) -0.0084(15) 0.0044(13) -0.0037(14) Si2 0.0324(15) 0.062(2) 0.0490(18) -0.0035(15) -0.0039(14) 0.0009(15) O1 0.037(4) 0.032(4) 0.043(4) -0.012(3) 0.009(3) 0.005(3) O2 0.031(3) 0.041(5) 0.053(4) 0.001(3) 0.007(3) 0.017(3) N1 0.031(4) 0.036(4) 0.043(4) -0.005(4) -0.004(4) 0.006(4) N2 0.034(5) 0.053(6) 0.041(5) 0.001(4) -0.011(4) -0.001(4) N3 0.050(5) 0.036(5) 0.049(5) -0.020(4) 0.004(5) -0.006(5) N4 0.028(4) 0.040(5) 0.043(5) -0.010(4) 0.005(4) 0.005(4) C1 0.015(4) 0.041(5) 0.051(6) 0.007(5) -0.003(4) -0.016(4) C2 0.041(6) 0.065(8) 0.033(6) -0.003(5) 0.008(5) -0.003(6) C3 0.044(6) 0.054(7) 0.056(7) 0.008(6) 0.005(7) 0.003(5) C4 0.045(7) 0.078(9) 0.043(6) -0.008(6) 0.000(6) -0.003(6) C5 0.040(6) 0.041(6) 0.041(6) -0.005(5) 0.001(5) 0.005(5) C6 0.031(6) 0.055(7) 0.035(5) 0.005(5) 0.001(4) 0.008(5) C7 0.042(6) 0.022(5) 0.091(9) -0.002(6) 0.010(6) -0.005(5) C8 0.084(9) 0.044(7) 0.064(8) 0.024(6) 0.016(8) 0.016(8) C9 0.060(8) 0.040(7) 0.074(9) 0.011(6) -0.010(7) 0.008(6) C10 0.035(6) 0.041(6) 0.069(8) -0.012(6) -0.020(6) -0.001(5) C11 0.039(6) 0.043(6) 0.040(6) 0.000(5) -0.002(5) -0.014(5) C12 0.036(6) 0.072(9) 0.046(7) 0.003(6) 0.007(5) -0.022(6) C13 0.041(6) 0.049(7) 0.048(6) -0.006(5) -0.002(5) -0.008(5) C14 0.055(8) 0.125(14) 0.039(7) -0.029(8) 0.006(6) -0.036(9) C15 0.052(7) 0.065(9) 0.075(9) -0.039(7) 0.006(7) -0.029(7) C16 0.071(8) 0.045(7) 0.089(10) -0.010(7) 0.002(8) 0.026(7) C17 0.062(8) 0.069(9) 0.056(7) -0.004(7) -0.001(6) -0.020(7) C18 0.167(19) 0.055(9) 0.068(9) -0.009(7) 0.036(11) 0.008(11) C19 0.049(6) 0.056(7) 0.061(7) -0.012(5) -0.009(7) 0.001(7) C20 0.065(9) 0.098(11) 0.050(7) -0.030(7) 0.006(7) 0.007(9) C21 0.040(7) 0.056(9) 0.111(12) -0.008(8) -0.011(7) -0.007(6) C22 0.037(6) 0.108(13) 0.100(11) -0.061(10) -0.012(7) 0.029(8) C23 0.063(8) 0.081(11) 0.074(9) 0.020(7) -0.016(8) -0.015(8) C24 0.032(5) 0.036(5) 0.037(5) 0.007(4) 0.007(4) -0.008(4) C25 0.035(5) 0.075(8) 0.032(5) -0.008(5) -0.003(5) 0.006(6) C26 0.048(6) 0.022(5) 0.047(6) -0.004(4) 0.009(5) -0.006(4) C27 0.044(6) 0.090(9) 0.029(5) -0.006(6) 0.004(5) -0.018(8) C28 0.047(6) 0.022(5) 0.039(5) 0.004(4) 0.007(5) 0.007(4) C29 0.028(5) 0.049(6) 0.030(5) -0.003(4) 0.003(4) -0.007(4) C30 0.046(6) 0.082(9) 0.043(7) 0.014(6) -0.009(5) -0.028(6) C31 0.130(15) 0.028(6) 0.064(8) -0.012(6) -0.003(9) -0.004(8) C32 0.040(6) 0.045(6) 0.083(9) 0.017(6) -0.016(7) -0.020(5) C33 0.080(9) 0.072(9) 0.091(10) 0.020(8) -0.032(9) -0.056(8) C34 0.062(8) 0.058(8) 0.060(7) 0.000(6) 0.012(6) -0.026(7) C35 0.029(5) 0.082(8) 0.034(5) 0.011(5) 0.003(5) 0.005(6) C36 0.057(8) 0.136(15) 0.051(8) 0.039(8) -0.007(7) -0.040(9) C37 0.023(5) 0.121(14) 0.070(9) 0.027(8) -0.001(6) -0.009(7) C38 0.069(9) 0.070(10) 0.065(8) -0.006(6) 0.023(7) -0.016(7) C39 0.027(5) 0.053(6) 0.037(5) -0.001(5) 0.003(4) 0.006(5) C40 0.043(6) 0.056(7) 0.032(5) -0.001(4) 0.002(5) -0.006(6) C41 0.037(5) 0.046(6) 0.046(6) -0.010(6) 0.006(6) 0.018(5) C42 0.032(5) 0.051(7) 0.036(5) 0.005(5) -0.002(5) 0.004(5) C43 0.023(4) 0.067(8) 0.039(5) 0.002(5) 0.007(4) -0.004(5) C44 0.030(4) 0.039(5) 0.039(5) -0.012(4) -0.003(6) 0.014(4) C45 0.051(7) 0.033(6) 0.059(7) -0.006(5) 0.021(6) 0.016(5) C46 0.108(11) 0.030(6) 0.114(12) 0.005(7) 0.054(10) -0.016(7) C47 0.044(7) 0.079(10) 0.072(9) 0.027(7) 0.020(6) 0.016(6) C48 0.052(7) 0.123(13) 0.071(9) 0.051(8) 0.005(8) 0.011(9) C49 0.041(7) 0.039(6) 0.061(7) 0.001(5) 0.010(5) 0.005(5) C50 0.027(5) 0.081(9) 0.044(7) -0.009(6) 0.003(5) 0.011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O1 2.066(7) . ? Yb1 O2 2.069(7) . ? Yb1 N2 2.259(9) . ? Yb1 N1 2.416(8) . ? Yb1 N4 2.417(8) . ? Yb1 C1 2.776(10) . ? Si1 N1 1.722(8) . ? Si1 C20 1.811(15) . ? Si1 C18 1.841(15) . ? Si1 C19 1.869(13) . ? Si2 N3 1.775(10) . ? Si2 C22 1.845(12) . ? Si2 C23 1.858(13) . ? Si2 C21 1.897(13) . ? O1 C24 1.389(12) . ? O2 C39 1.360(12) . ? N1 C1 1.356(13) . ? N2 C1 1.349(13) . ? N2 C3 1.454(15) . ? N3 C2 1.414(15) . ? N3 H3 0.859(10) . ? N4 C2 1.320(14) . ? N4 C5 1.506(12) . ? C1 C6 1.484(13) . ? C2 C12 1.431(16) . ? C3 C4 1.558(16) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.440(16) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C7 1.357(12) . ? C6 C11 1.377(12) . ? C7 C8 1.371(17) . ? C7 H7 0.9400 . ? C8 C9 1.375(14) . ? C8 H8 0.9400 . ? C9 C10 1.376(13) . ? C9 H9 0.9400 . ? C10 C11 1.392(15) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C17 1.322(18) . ? C12 C13 1.368(16) . ? C13 C14 1.409(17) . ? C13 H13 0.9400 . ? C14 C15 1.29(2) . ? C14 H14 0.9400 . ? C15 C16 1.404(19) . ? C15 H15 0.9400 . ? C16 C17 1.428(18) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C29 1.406(14) . ? C24 C25 1.432(15) . ? C25 C26 1.354(15) . ? C25 C30 1.543(14) . ? C26 C27 1.362(14) . ? C26 H26 0.9400 . ? C27 C28 1.352(15) . ? C27 C34 1.515(16) . ? C28 C29 1.419(14) . ? C28 H28 0.9400 . ? C29 C35 1.548(15) . ? C30 C31 1.521(18) . ? C30 C32 1.539(17) . ? C30 C33 1.552(15) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 C36 1.519(15) . ? C35 C37 1.534(16) . ? C35 C38 1.538(17) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 C44 1.387(15) . ? C39 C40 1.422(15) . ? C40 C41 1.398(15) . ? C40 C45 1.531(16) . ? C41 C42 1.384(15) . ? C41 H41 0.9400 . ? C42 C43 1.380(16) . ? C42 C49 1.520(14) . ? C43 C44 1.398(13) . ? C43 H43 0.9400 . ? C44 C50 1.517(14) . ? C45 C47 1.531(16) . ? C45 C48 1.569(17) . ? C45 C46 1.630(16) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C49 H49C 0.9700 . ? C50 C52 1.519(17) . ? C50 C53' 1.520(17) . ? C50 C52' 1.530(16) . ? C50 C53 1.539(17) . ? C50 C51 1.553(16) . ? C50 C51' 1.563(17) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C51' H51D 0.9700 . ? C51' H51E 0.9700 . ? C51' H51F 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52 H52C 0.9700 . ? C52' H52D 0.9700 . ? C52' H52E 0.9700 . ? C52' H52F 0.9700 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C53' H53D 0.9700 . ? C53' H53E 0.9700 . ? C53' H53F 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O2 126.7(3) . . ? O1 Yb1 N2 106.7(3) . . ? O2 Yb1 N2 126.4(3) . . ? O1 Yb1 N1 115.3(3) . . ? O2 Yb1 N1 97.7(3) . . ? N2 Yb1 N1 58.0(3) . . ? O1 Yb1 N4 94.0(3) . . ? O2 Yb1 N4 91.7(3) . . ? N2 Yb1 N4 79.6(3) . . ? N1 Yb1 N4 133.2(3) . . ? O1 Yb1 C1 114.7(3) . . ? O2 Yb1 C1 114.2(3) . . ? N2 Yb1 C1 28.8(3) . . ? N1 Yb1 C1 29.3(3) . . ? N4 Yb1 C1 106.3(3) . . ? N1 Si1 C20 105.3(5) . . ? N1 Si1 C18 115.9(6) . . ? C20 Si1 C18 102.5(7) . . ? N1 Si1 C19 114.2(5) . . ? C20 Si1 C19 110.0(6) . . ? C18 Si1 C19 108.1(8) . . ? N3 Si2 C22 104.1(5) . . ? N3 Si2 C23 110.6(6) . . ? C22 Si2 C23 112.1(8) . . ? N3 Si2 C21 112.1(5) . . ? C22 Si2 C21 109.1(7) . . ? C23 Si2 C21 108.9(7) . . ? C24 O1 Yb1 170.6(6) . . ? C39 O2 Yb1 164.9(6) . . ? C1 N1 Si1 125.5(7) . . ? C1 N1 Yb1 90.2(6) . . ? Si1 N1 Yb1 143.9(4) . . ? C1 N2 C3 121.9(9) . . ? C1 N2 Yb1 97.4(7) . . ? C3 N2 Yb1 140.5(7) . . ? C2 N3 Si2 128.9(7) . . ? C2 N3 H3 125(8) . . ? Si2 N3 H3 105(8) . . ? C2 N4 C5 115.2(8) . . ? C2 N4 Yb1 133.3(7) . . ? C5 N4 Yb1 111.4(6) . . ? N2 C1 N1 114.3(9) . . ? N2 C1 C6 120.4(10) . . ? N1 C1 C6 125.2(9) . . ? N2 C1 Yb1 53.8(5) . . ? N1 C1 Yb1 60.5(5) . . ? C6 C1 Yb1 174.2(8) . . ? N4 C2 N3 116.3(10) . . ? N4 C2 C12 124.3(10) . . ? N3 C2 C12 119.0(10) . . ? N2 C3 C4 108.7(9) . . ? N2 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? N2 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C5 C4 C3 115.0(11) . . ? C5 C4 H4A 108.5 . . ? C3 C4 H4A 108.5 . . ? C5 C4 H4B 108.5 . . ? C3 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C4 C5 N4 114.4(9) . . ? C4 C5 H5A 108.7 . . ? N4 C5 H5A 108.7 . . ? C4 C5 H5B 108.7 . . ? N4 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C7 C6 C11 117.4(10) . . ? C7 C6 C1 122.5(9) . . ? C11 C6 C1 120.0(9) . . ? C6 C7 C8 122.4(11) . . ? C6 C7 H7 118.8 . . ? C8 C7 H7 118.8 . . ? C9 C8 C7 119.3(11) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 120.5(11) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C11 117.9(10) . . ? C9 C10 H10 121.0 . . ? C11 C10 H10 121.0 . . ? C6 C11 C10 122.4(10) . . ? C6 C11 H11 118.8 . . ? C10 C11 H11 118.8 . . ? C17 C12 C13 117.3(12) . . ? C17 C12 C2 116.9(11) . . ? C13 C12 C2 125.6(12) . . ? C12 C13 C14 121.0(13) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 122.2(13) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? C14 C15 C16 118.4(12) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? C15 C16 C17 118.3(13) . . ? C15 C16 H16 120.9 . . ? C17 C16 H16 120.9 . . ? C12 C17 C16 122.1(13) . . ? C12 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O1 C24 C29 119.9(9) . . ? O1 C24 C25 119.4(9) . . ? C29 C24 C25 120.6(9) . . ? C26 C25 C24 117.3(9) . . ? C26 C25 C30 121.3(10) . . ? C24 C25 C30 121.4(10) . . ? C25 C26 C27 124.4(11) . . ? C25 C26 H26 117.8 . . ? C27 C26 H26 117.8 . . ? C28 C27 C26 118.1(11) . . ? C28 C27 C34 121.3(10) . . ? C26 C27 C34 120.6(10) . . ? C27 C28 C29 123.2(10) . . ? C27 C28 H28 118.4 . . ? C29 C28 H28 118.4 . . ? C24 C29 C28 116.3(9) . . ? C24 C29 C35 124.7(9) . . ? C28 C29 C35 118.9(9) . . ? C31 C30 C32 112.2(10) . . ? C31 C30 C25 109.3(11) . . ? C32 C30 C25 112.1(10) . . ? C31 C30 C33 105.5(12) . . ? C32 C30 C33 106.6(11) . . ? C25 C30 C33 111.0(10) . . ? 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 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C27 C34 H34A 109.5 . . ? C27 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C27 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C37 105.6(10) . . ? C36 C35 C38 108.1(11) . . ? C37 C35 C38 113.0(11) . . ? C36 C35 C29 111.9(10) . . ? C37 C35 C29 110.4(9) . . ? C38 C35 C29 107.9(10) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O2 C39 C44 122.3(9) . . ? O2 C39 C40 118.2(9) . . ? C44 C39 C40 119.2(9) . . ? C41 C40 C39 119.3(10) . . ? C41 C40 C45 115.8(10) . . ? C39 C40 C45 124.8(10) . . ? C42 C41 C40 121.4(10) . . ? C42 C41 H41 119.3 . . ? C40 C41 H41 119.3 . . ? C43 C42 C41 118.1(9) . . ? C43 C42 C49 121.7(10) . . ? C41 C42 C49 120.1(10) . . ? C42 C43 C44 122.5(10) . . ? C42 C43 H43 118.7 . . ? C44 C43 H43 118.7 . . ? C39 C44 C43 119.2(9) . . ? C39 C44 C50 123.1(9) . . ? C43 C44 C50 117.7(9) . . ? C40 C45 C47 122.4(10) . . ? C40 C45 C48 108.0(11) . . ? C47 C45 C48 106.7(10) . . ? C40 C45 C46 107.4(9) . . ? C47 C45 C46 101.7(11) . . ? C48 C45 C46 110.3(11) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C42 C49 H49A 109.5 . . ? C42 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C42 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C44 C50 C52 110.7(13) . . ? C44 C50 C53' 116.2(15) . . ? C52 C50 C53' 119.1(18) . . ? C44 C50 C52' 117.8(13) . . ? C52 C50 C52' 32.9(12) . . ? C53' C50 C52' 89.7(17) . . ? C44 C50 C53 115.9(14) . . ? C52 C50 C53 103.1(16) . . ? C53' C50 C53 20.6(14) . . ? C52' C50 C53 71.4(15) . . ? C44 C50 C51 110.5(12) . . ? C52 C50 C51 101.7(15) . . ? C53' C50 C51 96.1(16) . . ? C52' C50 C51 122.2(16) . . ? C53 C50 C51 113.7(16) . . ? C44 C50 C51' 113.8(12) . . ? C52 C50 C51' 59.6(14) . . ? C53' C50 C51' 124.5(17) . . ? C52' C50 C51' 87.4(16) . . ? C53 C50 C51' 130.2(17) . . ? C51 C50 C51' 43.5(12) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C51' H51D 109.5 . . ? C50 C51' H51E 109.5 . . ? H51D C51' H51E 109.5 . . ? C50 C51' H51F 109.5 . . ? H51D C51' H51F 109.5 . . ? H51E C51' H51F 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C52' H52D 109.5 . . ? C50 C52' H52E 109.5 . . ? H52D C52' H52E 109.5 . . ? C50 C52' H52F 109.5 . . ? H52D C52' H52F 109.5 . . ? H52E C52' H52F 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C50 C53' H53D 109.5 . . ? C50 C53' H53E 109.5 . . ? H53D C53' H53E 109.5 . . ? C50 C53' H53F 109.5 . . ? H53D C53' H53F 109.5 . . ? H53E C53' H53F 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 O2 Yb1 O1 C24 -62(4) . . . . ? N2 Yb1 O1 C24 123(4) . . . . ? N1 Yb1 O1 C24 61(4) . . . . ? N4 Yb1 O1 C24 -157(4) . . . . ? C1 Yb1 O1 C24 93(4) . . . . ? O1 Yb1 O2 C39 112(3) . . . . ? N2 Yb1 O2 C39 -74(3) . . . . ? N1 Yb1 O2 C39 -18(3) . . . . ? N4 Yb1 O2 C39 -152(3) . . . . ? C1 Yb1 O2 C39 -43(3) . . . . ? C20 Si1 N1 C1 179.3(9) . . . . ? C18 Si1 N1 C1 66.8(11) . . . . ? C19 Si1 N1 C1 -59.9(9) . . . . ? C20 Si1 N1 Yb1 8.9(10) . . . . ? C18 Si1 N1 Yb1 -103.6(10) . . . . ? C19 Si1 N1 Yb1 129.7(8) . . . . ? O1 Yb1 N1 C1 95.8(5) . . . . ? O2 Yb1 N1 C1 -127.2(5) . . . . ? N2 Yb1 N1 C1 1.2(5) . . . . ? N4 Yb1 N1 C1 -27.5(7) . . . . ? O1 Yb1 N1 Si1 -92.0(8) . . . . ? O2 Yb1 N1 Si1 45.0(8) . . . . ? N2 Yb1 N1 Si1 173.4(9) . . . . ? N4 Yb1 N1 Si1 144.7(7) . . . . ? C1 Yb1 N1 Si1 172.2(12) . . . . ? O1 Yb1 N2 C1 -111.0(6) . . . . ? O2 Yb1 N2 C1 73.5(7) . . . . ? N1 Yb1 N2 C1 -1.2(5) . . . . ? N4 Yb1 N2 C1 157.9(6) . . . . ? O1 Yb1 N2 C3 74.3(12) . . . . ? O2 Yb1 N2 C3 -101.2(12) . . . . ? N1 Yb1 N2 C3 -175.9(13) . . . . ? N4 Yb1 N2 C3 -16.8(11) . . . . ? C1 Yb1 N2 C3 -174.7(15) . . . . ? C22 Si2 N3 C2 -161.1(11) . . . . ? C23 Si2 N3 C2 78.3(12) . . . . ? C21 Si2 N3 C2 -43.3(12) . . . . ? O1 Yb1 N4 C2 108.7(10) . . . . ? O2 Yb1 N4 C2 -18.2(10) . . . . ? N2 Yb1 N4 C2 -145.0(11) . . . . ? N1 Yb1 N4 C2 -120.5(10) . . . . ? C1 Yb1 N4 C2 -134.1(10) . . . . ? O1 Yb1 N4 C5 -73.5(7) . . . . ? O2 Yb1 N4 C5 159.6(7) . . . . ? N2 Yb1 N4 C5 32.8(7) . . . . ? N1 Yb1 N4 C5 57.3(8) . . . . ? C1 Yb1 N4 C5 43.7(7) . . . . ? C3 N2 C1 N1 178.0(9) . . . . ? Yb1 N2 C1 N1 2.0(8) . . . . ? C3 N2 C1 C6 -4.1(14) . . . . ? Yb1 N2 C1 C6 179.9(7) . . . . ? C3 N2 C1 Yb1 176.0(11) . . . . ? Si1 N1 C1 N2 -176.2(7) . . . . ? Yb1 N1 C1 N2 -1.9(8) . . . . ? Si1 N1 C1 C6 6.0(13) . . . . ? Yb1 N1 C1 C6 -179.6(8) . . . . ? Si1 N1 C1 Yb1 -174.4(8) . . . . ? O1 Yb1 C1 N2 79.7(6) . . . . ? O2 Yb1 C1 N2 -122.2(6) . . . . ? N1 Yb1 C1 N2 177.9(9) . . . . ? N4 Yb1 C1 N2 -22.6(6) . . . . ? O1 Yb1 C1 N1 -98.2(6) . . . . ? O2 Yb1 C1 N1 59.9(6) . . . . ? N2 Yb1 C1 N1 -177.9(9) . . . . ? N4 Yb1 C1 N1 159.5(5) . . . . ? O1 Yb1 C1 C6 79(6) . . . . ? O2 Yb1 C1 C6 -123(6) . . . . ? N2 Yb1 C1 C6 -1(6) . . . . ? N1 Yb1 C1 C6 177(6) . . . . ? N4 Yb1 C1 C6 -24(6) . . . . ? C5 N4 C2 N3 178.6(9) . . . . ? Yb1 N4 C2 N3 -3.7(16) . . . . ? C5 N4 C2 C12 4.6(16) . . . . ? Yb1 N4 C2 C12 -177.6(8) . . . . ? Si2 N3 C2 N4 -175.9(8) . . . . ? Si2 N3 C2 C12 -1.6(16) . . . . ? C1 N2 C3 C4 -149.4(9) . . . . ? Yb1 N2 C3 C4 24.4(16) . . . . ? N2 C3 C4 C5 -49.8(13) . . . . ? C3 C4 C5 N4 85.3(12) . . . . ? C2 N4 C5 C4 104.4(12) . . . . ? Yb1 N4 C5 C4 -73.9(10) . . . . ? N2 C1 C6 C7 101.4(12) . . . . ? N1 C1 C6 C7 -81.0(14) . . . . ? Yb1 C1 C6 C7 103(6) . . . . ? N2 C1 C6 C11 -83.3(13) . . . . ? N1 C1 C6 C11 94.3(13) . . . . ? Yb1 C1 C6 C11 -82(6) . . . . ? C11 C6 C7 C8 2.1(18) . . . . ? C1 C6 C7 C8 177.5(11) . . . . ? C6 C7 C8 C9 -2(2) . . . . ? C7 C8 C9 C10 2(2) . . . . ? C8 C9 C10 C11 -1.5(19) . . . . ? C7 C6 C11 C10 -1.9(17) . . . . ? C1 C6 C11 C10 -177.4(10) . . . . ? C9 C10 C11 C6 1.6(17) . . . . ? N4 C2 C12 C17 -84.7(15) . . . . ? N3 C2 C12 C17 101.6(15) . . . . ? N4 C2 C12 C13 99.8(16) . . . . ? N3 C2 C12 C13 -74.0(15) . . . . ? C17 C12 C13 C14 4.0(18) . . . . ? C2 C12 C13 C14 179.6(12) . . . . ? C12 C13 C14 C15 -5(2) . . . . ? C13 C14 C15 C16 8(2) . . . . ? C14 C15 C16 C17 -9(2) . . . . ? C13 C12 C17 C16 -6(2) . . . . ? C2 C12 C17 C16 178.2(12) . . . . ? C15 C16 C17 C12 9(2) . . . . ? Yb1 O1 C24 C29 119(4) . . . . ? Yb1 O1 C24 C25 -63(4) . . . . ? O1 C24 C25 C26 -179.0(9) . . . . ? C29 C24 C25 C26 -1.3(16) . . . . ? O1 C24 C25 C30 0.7(16) . . . . ? C29 C24 C25 C30 178.4(10) . . . . ? C24 C25 C26 C27 -1.6(17) . . . . ? C30 C25 C26 C27 178.7(11) . . . . ? C25 C26 C27 C28 3.4(18) . . . . ? C25 C26 C27 C34 -174.0(11) . . . . ? C26 C27 C28 C29 -2.4(17) . . . . ? C34 C27 C28 C29 175.0(11) . . . . ? O1 C24 C29 C28 179.9(9) . . . . ? C25 C24 C29 C28 2.2(15) . . . . ? O1 C24 C29 C35 3.5(16) . . . . ? C25 C24 C29 C35 -174.2(10) . . . . ? C27 C28 C29 C24 -0.3(16) . . . . ? C27 C28 C29 C35 176.3(10) . . . . ? C26 C25 C30 C31 -114.5(12) . . . . ? C24 C25 C30 C31 65.8(14) . . . . ? C26 C25 C30 C32 120.5(11) . . . . ? C24 C25 C30 C32 -59.2(14) . . . . ? C26 C25 C30 C33 1.4(17) . . . . ? C24 C25 C30 C33 -178.3(12) . . . . ? C24 C29 C35 C36 -173.4(11) . . . . ? C28 C29 C35 C36 10.3(15) . . . . ? C24 C29 C35 C37 -56.0(15) . . . . ? C28 C29 C35 C37 127.7(11) . . . . ? C24 C29 C35 C38 67.8(13) . . . . ? C28 C29 C35 C38 -108.5(11) . . . . ? Yb1 O2 C39 C44 93(3) . . . . ? Yb1 O2 C39 C40 -93(3) . . . . ? O2 C39 C40 C41 -170.5(9) . . . . ? C44 C39 C40 C41 3.7(15) . . . . ? O2 C39 C40 C45 7.9(16) . . . . ? C44 C39 C40 C45 -177.9(10) . . . . ? C39 C40 C41 C42 0.1(16) . . . . ? C45 C40 C41 C42 -178.5(10) . . . . ? C40 C41 C42 C43 -3.6(16) . . . . ? C40 C41 C42 C49 178.2(10) . . . . ? C41 C42 C43 C44 3.5(15) . . . . ? C49 C42 C43 C44 -178.3(9) . . . . ? O2 C39 C44 C43 170.2(9) . . . . ? C40 C39 C44 C43 -3.8(15) . . . . ? O2 C39 C44 C50 -9.2(15) . . . . ? C40 C39 C44 C50 176.8(9) . . . . ? C42 C43 C44 C39 0.2(15) . . . . ? C42 C43 C44 C50 179.7(9) . . . . ? C41 C40 C45 C47 -161.8(11) . . . . ? C39 C40 C45 C47 19.7(18) . . . . ? C41 C40 C45 C48 73.8(12) . . . . ? C39 C40 C45 C48 -104.6(13) . . . . ? C41 C40 C45 C46 -45.1(14) . . . . ? C39 C40 C45 C46 136.5(12) . . . . ? C39 C44 C50 C52 115.3(14) . . . . ? C43 C44 C50 C52 -64.1(15) . . . . ? C39 C44 C50 C53' -24.7(18) . . . . ? C43 C44 C50 C53' 155.8(15) . . . . ? C39 C44 C50 C52' 79.9(17) . . . . ? C43 C44 C50 C52' -99.5(16) . . . . ? C39 C44 C50 C53 -1.7(18) . . . . ? C43 C44 C50 C53 178.8(13) . . . . ? C39 C44 C50 C51 -132.9(14) . . . . ? C43 C44 C50 C51 47.7(15) . . . . ? C39 C44 C50 C51' -179.9(13) . . . . ? C43 C44 C50 C51' 0.7(16) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.888 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.141 data_complex8 _database_code_depnum_ccdc_archive 'CCDC 915742' #TrackingRef '915742.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H78 N7 O Si2 Yb, C4 H8 O' _chemical_formula_sum 'C55 H86 N7 O2 Si2 Yb' _chemical_formula_weight 1106.53 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 13.980(2) _cell_length_b 26.110(3) _cell_length_c 17.139(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.891(4) _cell_angle_gamma 90.00 _cell_volume 5804.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 24694 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2316 _exptl_absorpt_coefficient_mu 1.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.290 _exptl_absorpt_correction_T_max 0.846 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28075 _diffrn_reflns_av_R_equivalents 0.1050 _diffrn_reflns_av_unetI/netI 0.1360 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10714 _reflns_number_gt 8132 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their N3-H3 and N7- H7A distances were constrained. ; _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^)+(0.0001P)^2^+19.6361P] 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 10714 _refine_ls_number_parameters 628 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1327 _refine_ls_R_factor_gt 0.0984 _refine_ls_wR_factor_ref 0.1558 _refine_ls_wR_factor_gt 0.1410 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.188 _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 Yb1 Yb 0.54260(3) 0.662531(15) 0.22625(3) 0.02718(13) Uani 1 1 d . . . Si1 Si 0.6212(2) 0.80385(10) 0.28109(17) 0.0345(7) Uani 1 1 d . . . Si2 Si 0.2171(3) 0.54839(12) 0.1948(2) 0.0478(8) Uani 1 1 d . . . O1 O 0.6672(5) 0.6127(2) 0.2531(4) 0.0329(16) Uani 1 1 d . . . O2 O 0.2244(7) 0.7954(3) 0.3387(6) 0.070(3) Uani 1 1 d . . . N1 N 0.5898(6) 0.7496(3) 0.2188(5) 0.0306(19) Uani 1 1 d . . . N2 N 0.5350(6) 0.7009(3) 0.1033(5) 0.0301(19) Uani 1 1 d . . . N3 N 0.3097(6) 0.5849(3) 0.1714(5) 0.037(2) Uani 1 1 d D . . H3 H 0.342(7) 0.610(3) 0.204(5) 0.055 Uiso 1 1 d D . . N4 N 0.4373(6) 0.6042(3) 0.1189(5) 0.0287(18) Uani 1 1 d . . . N5 N 0.5381(6) 0.6672(3) 0.3605(5) 0.0310(18) Uani 1 1 d . . . N6 N 0.3943(6) 0.6893(3) 0.2525(5) 0.0294(19) Uani 1 1 d . . . N7 N 0.4108(6) 0.7178(3) 0.3883(5) 0.033(2) Uani 1 1 d D . . H7A H 0.353(4) 0.735(3) 0.367(6) 0.050 Uiso 1 1 d D . . C1 C 0.5675(7) 0.7467(3) 0.1356(6) 0.028(2) Uani 1 1 d . . . C2 C 0.3515(7) 0.5798(4) 0.1110(6) 0.032(2) Uani 1 1 d . . . C3 C 0.5104(8) 0.6899(4) 0.0138(6) 0.038(3) Uani 1 1 d . . . H3A H 0.5741 0.6831 0.0041 0.046 Uiso 1 1 calc R . . H3B H 0.4765 0.7196 -0.0202 0.046 Uiso 1 1 calc R . . C4 C 0.4406(8) 0.6442(4) -0.0119(6) 0.036(2) Uani 1 1 d . . . H4A H 0.4377 0.6323 -0.0670 0.044 Uiso 1 1 calc R . . H4B H 0.3709 0.6546 -0.0178 0.044 Uiso 1 1 calc R . . C5 C 0.4743(7) 0.6002(4) 0.0496(6) 0.033(2) Uani 1 1 d . . . H5A H 0.4490 0.5681 0.0193 0.040 Uiso 1 1 calc R . . H5B H 0.5498 0.5987 0.0730 0.040 Uiso 1 1 calc R . . C6 C 0.5742(8) 0.7916(3) 0.0838(6) 0.030(2) Uani 1 1 d . . . C7 C 0.4929(8) 0.8249(4) 0.0498(6) 0.042(3) Uani 1 1 d . . . H7 H 0.4300 0.8183 0.0559 0.050 Uiso 1 1 calc R . . C8 C 0.5030(9) 0.8677(4) 0.0068(6) 0.045(3) Uani 1 1 d . . . H8 H 0.4475 0.8905 -0.0162 0.054 Uiso 1 1 calc R . . C9 C 0.5959(9) 0.8770(4) -0.0023(7) 0.047(3) Uani 1 1 d . . . H9 H 0.6034 0.9069 -0.0301 0.056 Uiso 1 1 calc R . . C10 C 0.6770(9) 0.8439(4) 0.0281(7) 0.054(3) Uani 1 1 d . . . H10 H 0.7389 0.8502 0.0202 0.064 Uiso 1 1 calc R . . C11 C 0.6661(9) 0.8004(4) 0.0712(7) 0.047(3) Uani 1 1 d . . . H11 H 0.7206 0.7769 0.0920 0.056 Uiso 1 1 calc R . . C12 C 0.2929(8) 0.5462(4) 0.0379(6) 0.035(2) Uani 1 1 d . . . C13 C 0.3275(9) 0.4981(4) 0.0280(8) 0.054(3) Uani 1 1 d . . . H13 H 0.3872 0.4848 0.0699 0.065 Uiso 1 1 calc R . . C14 C 0.2756(9) 0.4690(4) -0.0428(8) 0.058(4) Uani 1 1 d . . . H14 H 0.2994 0.4361 -0.0484 0.070 Uiso 1 1 calc R . . C15 C 0.1890(10) 0.4885(5) -0.1050(8) 0.061(4) Uani 1 1 d . . . H15 H 0.1540 0.4693 -0.1537 0.073 Uiso 1 1 calc R . . C16 C 0.1544(9) 0.5363(5) -0.0949(8) 0.064(4) Uani 1 1 d . . . H16 H 0.0947 0.5498 -0.1364 0.077 Uiso 1 1 calc R . . C17 C 0.2072(9) 0.5644(4) -0.0242(7) 0.057(3) Uani 1 1 d . . . H17 H 0.1832 0.5973 -0.0186 0.068 Uiso 1 1 calc R . . C18 C 0.7098(9) 0.8503(4) 0.2608(7) 0.052(3) Uani 1 1 d . . . H18A H 0.7691 0.8322 0.2580 0.078 Uiso 1 1 calc R . . H18B H 0.7326 0.8753 0.3059 0.078 Uiso 1 1 calc R . . H18C H 0.6740 0.8677 0.2078 0.078 Uiso 1 1 calc R . . C19 C 0.6864(8) 0.7811(4) 0.3909(6) 0.044(3) Uani 1 1 d . . . H19A H 0.6499 0.7516 0.4004 0.066 Uiso 1 1 calc R . . H19B H 0.6867 0.8082 0.4296 0.066 Uiso 1 1 calc R . . H19C H 0.7568 0.7714 0.4001 0.066 Uiso 1 1 calc R . . C20 C 0.4990(9) 0.8399(4) 0.2686(7) 0.057(3) Uani 1 1 d . . . H20A H 0.4729 0.8566 0.2141 0.085 Uiso 1 1 calc R . . H20B H 0.5138 0.8655 0.3125 0.085 Uiso 1 1 calc R . . H20C H 0.4478 0.8162 0.2727 0.085 Uiso 1 1 calc R . . C21 C 0.0825(9) 0.5635(5) 0.1222(9) 0.075(4) Uani 1 1 d . . . H21A H 0.0771 0.5997 0.1088 0.112 Uiso 1 1 calc R . . H21B H 0.0348 0.5548 0.1492 0.112 Uiso 1 1 calc R . . H21C H 0.0658 0.5437 0.0709 0.112 Uiso 1 1 calc R . . C22 C 0.2414(10) 0.5679(5) 0.3048(7) 0.066(4) Uani 1 1 d . . . H22A H 0.3138 0.5630 0.3391 0.100 Uiso 1 1 calc R . . H22B H 0.1997 0.5472 0.3269 0.100 Uiso 1 1 calc R . . H22C H 0.2235 0.6037 0.3059 0.100 Uiso 1 1 calc R . . C23 C 0.2393(11) 0.4788(4) 0.1888(8) 0.073(4) Uani 1 1 d . . . H23A H 0.2208 0.4689 0.1304 0.110 Uiso 1 1 calc R . . H23B H 0.1973 0.4600 0.2130 0.110 Uiso 1 1 calc R . . H23C H 0.3115 0.4712 0.2198 0.110 Uiso 1 1 calc R . . C24 C 0.7521(8) 0.5826(4) 0.2815(6) 0.033(2) Uani 1 1 d . . . C25 C 0.7460(8) 0.5320(4) 0.3084(6) 0.036(2) Uani 1 1 d . . . C26 C 0.8355(8) 0.5021(3) 0.3383(7) 0.038(3) Uani 1 1 d . . . H26 H 0.8315 0.4686 0.3570 0.046 Uiso 1 1 calc R . . C27 C 0.9292(8) 0.5202(3) 0.3412(6) 0.035(2) Uani 1 1 d . . . C28 C 0.9340(7) 0.5690(4) 0.3123(6) 0.033(2) Uani 1 1 d . . . H28 H 0.9974 0.5812 0.3126 0.040 Uiso 1 1 calc R . . C29 C 0.8478(7) 0.6010(3) 0.2827(5) 0.027(2) Uani 1 1 d . . . C30 C 0.6465(8) 0.5040(4) 0.3009(7) 0.038(3) Uani 1 1 d . . . C31 C 0.6630(10) 0.4523(4) 0.3467(9) 0.074(4) Uani 1 1 d . . . H31A H 0.6981 0.4290 0.3222 0.111 Uiso 1 1 calc R . . H31B H 0.5967 0.4379 0.3411 0.111 Uiso 1 1 calc R . . H31C H 0.7045 0.4572 0.4058 0.111 Uiso 1 1 calc R . . C32 C 0.5877(9) 0.4919(5) 0.2064(7) 0.065(4) Uani 1 1 d . . . H32A H 0.5814 0.5229 0.1736 0.098 Uiso 1 1 calc R . . H32B H 0.5195 0.4790 0.1981 0.098 Uiso 1 1 calc R . . H32C H 0.6253 0.4663 0.1884 0.098 Uiso 1 1 calc R . . C33 C 0.5754(9) 0.5353(4) 0.3332(9) 0.067(4) Uani 1 1 d . . . H33A H 0.6111 0.5426 0.3926 0.100 Uiso 1 1 calc R . . H33B H 0.5135 0.5157 0.3253 0.100 Uiso 1 1 calc R . . H33C H 0.5569 0.5672 0.3022 0.100 Uiso 1 1 calc R . . C34 C 1.0276(9) 0.4867(4) 0.3755(8) 0.061(4) Uani 1 1 d . . . H34A H 1.0678 0.4913 0.3405 0.092 Uiso 1 1 calc R . . H34B H 1.0082 0.4510 0.3747 0.092 Uiso 1 1 calc R . . H34C H 1.0684 0.4969 0.4327 0.092 Uiso 1 1 calc R . . C35 C 0.8595(7) 0.6545(4) 0.2501(6) 0.034(2) Uani 1 1 d . . . C36 C 0.9703(8) 0.6661(4) 0.2553(7) 0.050(3) Uani 1 1 d . . . H36A H 0.9922 0.6396 0.2260 0.074 Uiso 1 1 calc R . . H36B H 1.0167 0.6669 0.3138 0.074 Uiso 1 1 calc R . . H36C H 0.9714 0.6990 0.2295 0.074 Uiso 1 1 calc R . . C37 C 0.8360(8) 0.6960(4) 0.3046(7) 0.044(3) Uani 1 1 d . . . H37A H 0.8392 0.7296 0.2815 0.065 Uiso 1 1 calc R . . H37B H 0.8864 0.6940 0.3616 0.065 Uiso 1 1 calc R . . H37C H 0.7675 0.6905 0.3050 0.065 Uiso 1 1 calc R . . C38 C 0.7901(7) 0.6606(4) 0.1577(6) 0.040(2) Uani 1 1 d . . . H38A H 0.8102 0.6361 0.1241 0.060 Uiso 1 1 calc R . . H38B H 0.7969 0.6951 0.1392 0.060 Uiso 1 1 calc R . . H38C H 0.7189 0.6546 0.1509 0.060 Uiso 1 1 calc R . . C39 C 0.5830(8) 0.6428(3) 0.4380(6) 0.035(2) Uani 1 1 d . . . C40 C 0.5270(9) 0.6158(4) 0.4775(7) 0.044(3) Uani 1 1 d . . . H40 H 0.4546 0.6170 0.4549 0.053 Uiso 1 1 calc R . . C41 C 0.5772(11) 0.5869(5) 0.5500(8) 0.067(4) Uani 1 1 d . . . H41 H 0.5389 0.5695 0.5766 0.080 Uiso 1 1 calc R . . C42 C 0.6831(11) 0.5842(5) 0.5822(7) 0.068(4) Uani 1 1 d . . . H42 H 0.7169 0.5649 0.6311 0.081 Uiso 1 1 calc R . . C43 C 0.7403(10) 0.6095(5) 0.5434(8) 0.064(4) Uani 1 1 d . . . H43 H 0.8126 0.6068 0.5653 0.077 Uiso 1 1 calc R . . C44 C 0.6913(8) 0.6386(4) 0.4725(6) 0.042(3) Uani 1 1 d . . . H44 H 0.7307 0.6560 0.4469 0.051 Uiso 1 1 calc R . . C45 C 0.4470(8) 0.6913(4) 0.3364(6) 0.035(2) Uani 1 1 d . . . C46 C 0.3051(7) 0.7231(4) 0.2117(6) 0.032(2) Uani 1 1 d . . . H46 H 0.3186 0.7564 0.2416 0.039 Uiso 1 1 calc R . . C47 C 0.2941(8) 0.7323(4) 0.1217(6) 0.045(3) Uani 1 1 d . . . H47A H 0.3552 0.7495 0.1208 0.067 Uiso 1 1 calc R . . H47B H 0.2341 0.7535 0.0938 0.067 Uiso 1 1 calc R . . H47C H 0.2860 0.6997 0.0926 0.067 Uiso 1 1 calc R . . C48 C 0.2049(8) 0.7016(4) 0.2130(7) 0.045(3) Uani 1 1 d . . . H48A H 0.1879 0.6703 0.1803 0.067 Uiso 1 1 calc R . . H48B H 0.1502 0.7264 0.1890 0.067 Uiso 1 1 calc R . . H48C H 0.2127 0.6944 0.2706 0.067 Uiso 1 1 calc R . . C49 C 0.4701(8) 0.7383(4) 0.4738(6) 0.038(3) Uani 1 1 d . . . H49 H 0.5407 0.7238 0.4931 0.046 Uiso 1 1 calc R . . C50 C 0.4213(10) 0.7220(5) 0.5348(7) 0.062(4) Uani 1 1 d . . . H50A H 0.3518 0.7356 0.5167 0.092 Uiso 1 1 calc R . . H50B H 0.4617 0.7351 0.5904 0.092 Uiso 1 1 calc R . . H50C H 0.4190 0.6849 0.5367 0.092 Uiso 1 1 calc R . . C51 C 0.4782(9) 0.7959(4) 0.4718(7) 0.053(3) Uani 1 1 d . . . H51A H 0.4997 0.8058 0.4263 0.080 Uiso 1 1 calc R . . H51B H 0.5285 0.8078 0.5248 0.080 Uiso 1 1 calc R . . H51C H 0.4116 0.8110 0.4629 0.080 Uiso 1 1 calc R . . C52 C 0.2046(14) 0.8392(6) 0.2895(14) 0.133(8) Uani 1 1 d . . . H52A H 0.2102 0.8315 0.2354 0.160 Uiso 1 1 calc R . . H52B H 0.2552 0.8657 0.3178 0.160 Uiso 1 1 calc R . . C53 C 0.1008(14) 0.8574(6) 0.2758(15) 0.143(9) Uani 1 1 d . . . H53A H 0.1035 0.8904 0.3038 0.172 Uiso 1 1 calc R . . H53B H 0.0603 0.8615 0.2156 0.172 Uiso 1 1 calc R . . C54 C 0.0569(13) 0.8187(7) 0.3116(12) 0.117(7) Uani 1 1 d . . . H54A H 0.0084 0.7975 0.2672 0.141 Uiso 1 1 calc R . . H54B H 0.0197 0.8345 0.3439 0.141 Uiso 1 1 calc R . . C55 C 0.1444(12) 0.7868(7) 0.3680(10) 0.098(6) Uani 1 1 d . . . H55A H 0.1647 0.7975 0.4267 0.118 Uiso 1 1 calc R . . H55B H 0.1254 0.7504 0.3635 0.118 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 0.0262(2) 0.0267(2) 0.0276(2) 0.0000(2) 0.00895(17) 0.0007(2) Si1 0.0379(17) 0.0302(15) 0.0332(15) -0.0027(13) 0.0107(13) -0.0067(13) Si2 0.053(2) 0.0409(18) 0.061(2) -0.0030(17) 0.0341(18) -0.0095(16) O1 0.030(4) 0.032(4) 0.041(4) 0.001(3) 0.017(3) 0.005(3) O2 0.066(6) 0.067(6) 0.088(7) -0.005(5) 0.041(6) 0.016(5) N1 0.039(5) 0.029(4) 0.028(4) 0.003(4) 0.018(4) 0.004(4) N2 0.036(5) 0.027(4) 0.028(4) -0.003(4) 0.012(4) -0.007(4) N3 0.033(5) 0.034(5) 0.042(5) -0.007(4) 0.013(4) -0.012(4) N4 0.020(4) 0.038(5) 0.035(5) -0.004(4) 0.017(4) -0.007(4) N5 0.026(4) 0.037(5) 0.032(4) 0.003(4) 0.014(4) 0.010(4) N6 0.030(5) 0.032(4) 0.028(4) -0.004(4) 0.012(4) -0.006(4) N7 0.016(4) 0.050(5) 0.029(4) -0.002(4) 0.003(4) 0.001(4) C1 0.026(5) 0.030(5) 0.033(5) 0.000(5) 0.014(4) 0.003(4) C2 0.030(6) 0.028(5) 0.041(6) 0.000(5) 0.017(5) 0.011(5) C3 0.049(7) 0.037(6) 0.033(6) 0.003(5) 0.021(5) 0.005(5) C4 0.031(6) 0.043(6) 0.040(6) -0.010(5) 0.018(5) -0.002(5) C5 0.025(5) 0.034(6) 0.045(6) -0.008(5) 0.018(5) -0.006(5) C6 0.035(6) 0.023(5) 0.030(5) 0.002(4) 0.010(5) -0.002(4) C7 0.044(7) 0.036(6) 0.051(7) -0.004(5) 0.024(6) 0.001(5) C8 0.058(8) 0.025(6) 0.042(6) 0.010(5) 0.008(6) 0.005(5) C9 0.060(8) 0.034(6) 0.048(7) 0.018(5) 0.023(6) 0.000(6) C10 0.055(8) 0.050(7) 0.060(8) 0.007(7) 0.027(6) -0.011(7) C11 0.052(8) 0.032(6) 0.058(7) 0.010(6) 0.023(6) 0.006(5) C12 0.033(6) 0.034(6) 0.038(6) -0.006(5) 0.012(5) -0.012(5) C13 0.046(7) 0.037(6) 0.069(8) -0.021(6) 0.010(6) -0.007(6) C14 0.042(7) 0.051(7) 0.091(10) -0.032(7) 0.035(7) -0.015(6) C15 0.056(9) 0.073(9) 0.046(7) -0.019(7) 0.010(6) -0.021(8) C16 0.050(8) 0.061(9) 0.051(8) 0.013(7) -0.015(6) -0.018(7) C17 0.054(8) 0.042(7) 0.060(8) -0.003(6) 0.006(7) -0.011(6) C18 0.063(8) 0.050(7) 0.044(7) -0.007(6) 0.021(6) -0.031(6) C19 0.044(7) 0.043(6) 0.041(6) -0.012(5) 0.010(5) -0.005(5) C20 0.072(9) 0.044(6) 0.059(7) -0.003(6) 0.030(7) 0.015(7) C21 0.040(8) 0.087(10) 0.101(11) -0.024(9) 0.031(8) -0.013(7) C22 0.078(10) 0.073(9) 0.066(9) -0.007(7) 0.047(8) -0.025(8) C23 0.104(12) 0.055(8) 0.084(10) 0.006(8) 0.061(9) -0.002(8) C24 0.038(6) 0.032(5) 0.032(5) -0.004(5) 0.015(5) 0.002(5) C25 0.039(6) 0.032(5) 0.036(6) -0.002(5) 0.011(5) 0.002(5) C26 0.040(6) 0.020(5) 0.064(7) 0.010(5) 0.029(6) 0.002(5) C27 0.034(6) 0.025(5) 0.046(6) -0.003(5) 0.014(5) 0.005(5) C28 0.023(5) 0.037(6) 0.041(6) -0.011(5) 0.014(5) -0.005(5) C29 0.029(6) 0.029(5) 0.024(5) -0.008(4) 0.009(4) -0.006(4) C30 0.029(6) 0.039(6) 0.055(7) -0.005(5) 0.025(5) -0.003(5) C31 0.064(9) 0.051(8) 0.109(12) 0.033(8) 0.036(9) -0.002(7) C32 0.040(7) 0.079(9) 0.067(9) -0.011(8) 0.009(6) -0.011(7) C33 0.063(9) 0.037(6) 0.130(13) -0.003(7) 0.071(9) 0.002(6) C34 0.046(7) 0.036(6) 0.098(10) 0.015(7) 0.022(7) 0.003(6) C35 0.026(5) 0.028(5) 0.045(6) -0.003(5) 0.008(5) -0.004(5) C36 0.044(7) 0.039(6) 0.064(8) 0.001(6) 0.018(6) 0.001(6) C37 0.036(6) 0.033(6) 0.063(7) -0.005(6) 0.020(6) -0.001(5) C38 0.032(6) 0.045(6) 0.039(6) 0.007(6) 0.008(5) -0.003(5) C39 0.031(6) 0.027(5) 0.040(6) -0.008(5) 0.007(5) -0.001(5) C40 0.050(7) 0.042(6) 0.045(7) 0.004(6) 0.024(6) 0.000(6) C41 0.087(11) 0.070(9) 0.051(8) 0.012(7) 0.035(8) 0.007(8) C42 0.082(11) 0.073(9) 0.039(7) 0.034(7) 0.011(7) 0.020(8) C43 0.051(8) 0.068(9) 0.057(8) 0.026(7) 0.002(7) 0.012(7) C44 0.036(6) 0.049(7) 0.037(6) 0.007(5) 0.008(5) 0.007(5) C45 0.033(6) 0.037(6) 0.041(6) 0.004(5) 0.022(5) -0.005(5) C46 0.030(6) 0.036(6) 0.027(5) -0.010(5) 0.006(4) -0.005(5) C47 0.037(6) 0.064(8) 0.030(6) 0.013(6) 0.008(5) 0.017(6) C48 0.035(6) 0.037(6) 0.061(7) -0.007(6) 0.017(6) 0.000(5) C49 0.039(6) 0.049(7) 0.029(5) -0.013(5) 0.016(5) 0.002(5) C50 0.071(9) 0.082(9) 0.033(6) 0.005(6) 0.021(6) -0.007(8) C51 0.050(8) 0.055(7) 0.047(7) -0.001(6) 0.010(6) 0.003(6) C52 0.119(15) 0.057(10) 0.25(2) 0.051(14) 0.099(17) 0.043(11) C53 0.091(14) 0.084(13) 0.27(3) 0.052(15) 0.082(17) 0.005(11) C54 0.075(12) 0.154(18) 0.144(17) 0.034(14) 0.064(12) 0.035(12) C55 0.090(13) 0.139(15) 0.081(11) 0.032(11) 0.051(10) 0.047(11) _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 O1 2.083(6) . ? Yb1 N2 2.300(7) . ? Yb1 N5 2.328(7) . ? Yb1 N1 2.384(7) . ? Yb1 N6 2.384(8) . ? Yb1 N4 2.419(7) . ? Yb1 C1 2.787(9) . ? Yb1 C45 2.792(10) . ? Si1 N1 1.728(8) . ? Si1 C18 1.857(10) . ? Si1 C19 1.857(10) . ? Si1 C20 1.891(11) . ? Si2 N3 1.769(9) . ? Si2 C23 1.851(12) . ? Si2 C22 1.859(12) . ? Si2 C21 1.871(12) . ? O1 C24 1.353(11) . ? O2 C52 1.384(16) . ? O2 C55 1.405(15) . ? N1 C1 1.345(11) . ? N2 C1 1.324(11) . ? N2 C3 1.471(11) . ? N3 H3 0.870(10) . ? N3 C2 1.372(12) . ? N3 H3 0.870(10) . ? N4 C2 1.320(11) . ? N4 C5 1.466(11) . ? N5 C45 1.340(11) . ? N5 C39 1.394(12) . ? N6 C45 1.350(12) . ? N6 C46 1.474(11) . ? N7 C45 1.364(12) . ? N7 C49 1.488(11) . ? N7 H7A 0.869(10) . ? C1 C6 1.495(12) . ? C2 C12 1.500(13) . ? C3 C4 1.501(13) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.510(13) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C7 1.375(13) . ? C6 C11 1.398(14) . ? C7 C8 1.376(13) . ? C7 H7 0.9400 . ? C8 C9 1.386(15) . ? C8 H8 0.9400 . ? C9 C10 1.365(15) . ? C9 H9 0.9400 . ? C10 C11 1.393(14) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C17 1.357(14) . ? C12 C13 1.379(13) . ? C13 C14 1.385(15) . ? C13 H13 0.9400 . ? C14 C15 1.378(16) . ? C14 H14 0.9400 . ? C15 C16 1.373(16) . ? C15 H15 0.9400 . ? C16 C17 1.372(15) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C25 1.413(13) . ? C24 C29 1.415(13) . ? C25 C26 1.400(13) . ? C25 C30 1.534(13) . ? C26 C27 1.377(13) . ? C26 H26 0.9400 . ? C27 C28 1.378(13) . ? C27 C34 1.548(13) . ? C28 C29 1.396(12) . ? C28 H28 0.9400 . ? C29 C35 1.535(12) . ? C30 C31 1.537(14) . ? C30 C33 1.539(13) . ? C30 C32 1.551(14) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 C38 1.527(12) . ? C35 C37 1.545(13) . ? C35 C36 1.548(13) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 C40 1.401(14) . ? C39 C44 1.409(13) . ? C40 C41 1.397(15) . ? C40 H40 0.9400 . ? C41 C42 1.375(17) . ? C41 H41 0.9400 . ? C42 C43 1.384(17) . ? C42 H42 0.9400 . ? C43 C44 1.380(14) . ? C43 H43 0.9400 . ? C44 H44 0.9400 . ? C46 C47 1.513(12) . ? C46 C48 1.516(13) . ? C46 H46 0.9900 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 C50 1.508(14) . ? C49 C51 1.510(13) . ? C49 H49 0.9900 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C50 H50C 0.9700 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C52 C53 1.46(2) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.44(2) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.498(19) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 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 O1 Yb1 N2 102.9(3) . . ? O1 Yb1 N5 98.2(2) . . ? N2 Yb1 N5 150.9(3) . . ? O1 Yb1 N1 112.5(3) . . ? N2 Yb1 N1 57.0(2) . . ? N5 Yb1 N1 96.4(3) . . ? O1 Yb1 N6 148.8(2) . . ? N2 Yb1 N6 107.4(3) . . ? N5 Yb1 N6 56.8(3) . . ? N1 Yb1 N6 90.5(3) . . ? O1 Yb1 N4 89.8(2) . . ? N2 Yb1 N4 76.7(3) . . ? N5 Yb1 N4 123.5(3) . . ? N1 Yb1 N4 131.5(3) . . ? N6 Yb1 N4 90.1(2) . . ? O1 Yb1 C1 110.3(3) . . ? N2 Yb1 C1 28.1(2) . . ? N5 Yb1 C1 124.4(3) . . ? N1 Yb1 C1 28.8(2) . . ? N6 Yb1 C1 99.9(3) . . ? N4 Yb1 C1 103.9(3) . . ? O1 Yb1 C45 126.2(3) . . ? N2 Yb1 C45 129.2(3) . . ? N5 Yb1 C45 28.6(3) . . ? N1 Yb1 C45 89.5(3) . . ? N6 Yb1 C45 28.9(3) . . ? N4 Yb1 C45 112.0(3) . . ? C1 Yb1 C45 110.8(3) . . ? N1 Si1 C18 116.9(5) . . ? N1 Si1 C19 106.2(4) . . ? C18 Si1 C19 106.8(5) . . ? N1 Si1 C20 109.1(5) . . ? C18 Si1 C20 106.9(5) . . ? C19 Si1 C20 110.9(5) . . ? N3 Si2 C23 111.3(5) . . ? N3 Si2 C22 102.1(5) . . ? C23 Si2 C22 110.8(6) . . ? N3 Si2 C21 112.0(5) . . ? C23 Si2 C21 108.5(6) . . ? C22 Si2 C21 112.0(6) . . ? C24 O1 Yb1 172.2(6) . . ? C52 O2 C55 110.2(11) . . ? C1 N1 Si1 127.4(6) . . ? C1 N1 Yb1 92.5(6) . . ? Si1 N1 Yb1 139.5(4) . . ? C1 N2 C3 121.5(8) . . ? C1 N2 Yb1 96.8(6) . . ? C3 N2 Yb1 141.6(6) . . ? H3 N3 C2 107(7) . . ? H3 N3 Si2 120(7) . . ? C2 N3 Si2 132.2(7) . . ? H3 N3 H3 0(6) . . ? C2 N3 H3 107(7) . . ? Si2 N3 H3 120(7) . . ? C2 N4 C5 117.7(8) . . ? C2 N4 Yb1 130.8(6) . . ? C5 N4 Yb1 111.2(5) . . ? C45 N5 C39 123.1(8) . . ? C45 N5 Yb1 95.3(6) . . ? C39 N5 Yb1 138.5(6) . . ? C45 N6 C46 120.6(8) . . ? C45 N6 Yb1 92.6(6) . . ? C46 N6 Yb1 136.7(6) . . ? C45 N7 C49 128.2(8) . . ? C45 N7 H7A 119(7) . . ? C49 N7 H7A 109(7) . . ? N2 C1 N1 113.7(8) . . ? N2 C1 C6 123.2(8) . . ? N1 C1 C6 123.0(8) . . ? N2 C1 Yb1 55.0(5) . . ? N1 C1 Yb1 58.7(5) . . ? C6 C1 Yb1 176.6(7) . . ? N4 C2 N3 120.2(9) . . ? N4 C2 C12 124.1(9) . . ? N3 C2 C12 115.7(9) . . ? N2 C3 C4 109.5(8) . . ? N2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? N2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C3 C4 C5 113.7(8) . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4B 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? N4 C5 C4 113.5(8) . . ? N4 C5 H5A 108.9 . . ? C4 C5 H5A 108.9 . . ? N4 C5 H5B 108.9 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C7 C6 C11 119.5(9) . . ? C7 C6 C1 121.6(9) . . ? C11 C6 C1 119.0(9) . . ? C6 C7 C8 120.5(10) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C7 C8 C9 119.3(10) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C10 C9 C8 121.8(10) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C9 C10 C11 118.6(11) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C10 C11 C6 120.3(10) . . ? C10 C11 H11 119.9 . . ? C6 C11 H11 119.9 . . ? C17 C12 C13 118.1(10) . . ? C17 C12 C2 119.8(9) . . ? C13 C12 C2 121.9(10) . . ? C12 C13 C14 120.8(11) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 119.9(11) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 119.2(11) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 119.9(12) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C12 C17 C16 122.1(11) . . ? C12 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O1 C24 C25 120.6(9) . . ? O1 C24 C29 120.4(8) . . ? C25 C24 C29 119.0(9) . . ? C26 C25 C24 119.2(9) . . ? C26 C25 C30 115.1(8) . . ? C24 C25 C30 125.5(9) . . ? C27 C26 C25 122.0(9) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C28 118.6(9) . . ? C26 C27 C34 121.2(9) . . ? C28 C27 C34 120.3(9) . . ? C27 C28 C29 122.2(9) . . ? C27 C28 H28 118.9 . . ? C29 C28 H28 118.9 . . ? C28 C29 C24 119.1(9) . . ? C28 C29 C35 118.8(8) . . ? C24 C29 C35 122.1(8) . . ? C25 C30 C31 114.6(9) . . ? C25 C30 C33 113.9(9) . . ? C31 C30 C33 106.0(9) . . ? C25 C30 C32 107.2(9) . . ? C31 C30 C32 106.0(9) . . ? C33 C30 C32 108.8(10) . . ? 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 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C27 C34 H34A 109.5 . . ? C27 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C27 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C38 C35 C29 111.1(8) . . ? C38 C35 C37 111.0(8) . . ? C29 C35 C37 110.1(8) . . ? C38 C35 C36 106.0(8) . . ? C29 C35 C36 113.4(8) . . ? C37 C35 C36 105.2(8) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N5 C39 C40 123.9(9) . . ? N5 C39 C44 117.8(9) . . ? C40 C39 C44 117.6(10) . . ? C41 C40 C39 121.0(11) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C42 C41 C40 119.6(12) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C41 C42 C43 120.7(11) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C44 C43 C42 119.9(12) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C39 121.1(11) . . ? C43 C44 H44 119.5 . . ? C39 C44 H44 119.5 . . ? N5 C45 N6 112.9(9) . . ? N5 C45 N7 125.3(9) . . ? N6 C45 N7 121.8(9) . . ? N5 C45 Yb1 56.1(5) . . ? N6 C45 Yb1 58.5(5) . . ? N7 C45 Yb1 164.8(7) . . ? N6 C46 C47 108.9(8) . . ? N6 C46 C48 113.2(8) . . ? C47 C46 C48 109.3(8) . . ? N6 C46 H46 108.4 . . ? C47 C46 H46 108.4 . . ? C48 C46 H46 108.4 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N7 C49 C50 110.6(9) . . ? N7 C49 C51 110.8(8) . . ? C50 C49 C51 110.6(9) . . ? N7 C49 H49 108.2 . . ? C50 C49 H49 108.2 . . ? C51 C49 H49 108.2 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O2 C52 C53 109.2(15) . . ? O2 C52 H52A 109.8 . . ? C53 C52 H52A 109.8 . . ? O2 C52 H52B 109.8 . . ? C53 C52 H52B 109.8 . . ? H52A C52 H52B 108.3 . . ? C54 C53 C52 105.0(15) . . ? C54 C53 H53A 110.7 . . ? C52 C53 H53A 110.7 . . ? C54 C53 H53B 110.7 . . ? C52 C53 H53B 110.7 . . ? H53A C53 H53B 108.8 . . ? C53 C54 C55 106.9(15) . . ? C53 C54 H54A 110.3 . . ? C55 C54 H54A 110.3 . . ? C53 C54 H54B 110.3 . . ? C55 C54 H54B 110.3 . . ? H54A C54 H54B 108.6 . . ? O2 C55 C54 104.3(12) . . ? O2 C55 H55A 110.9 . . ? C54 C55 H55A 110.9 . . ? O2 C55 H55B 110.9 . . ? C54 C55 H55B 110.9 . . ? H55A C55 H55B 108.9 . . ? 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 N2 Yb1 O1 C24 136(4) . . . . ? N5 Yb1 O1 C24 -24(5) . . . . ? N1 Yb1 O1 C24 77(5) . . . . ? N6 Yb1 O1 C24 -58(5) . . . . ? N4 Yb1 O1 C24 -148(5) . . . . ? C1 Yb1 O1 C24 108(4) . . . . ? C45 Yb1 O1 C24 -30(5) . . . . ? C18 Si1 N1 C1 -41.6(10) . . . . ? C19 Si1 N1 C1 -160.6(8) . . . . ? C20 Si1 N1 C1 79.8(9) . . . . ? C18 Si1 N1 Yb1 150.8(6) . . . . ? C19 Si1 N1 Yb1 31.8(8) . . . . ? C20 Si1 N1 Yb1 -87.8(7) . . . . ? O1 Yb1 N1 C1 91.6(6) . . . . ? N2 Yb1 N1 C1 0.5(5) . . . . ? N5 Yb1 N1 C1 -166.7(5) . . . . ? N6 Yb1 N1 C1 -110.1(6) . . . . ? N4 Yb1 N1 C1 -19.5(7) . . . . ? C45 Yb1 N1 C1 -139.0(6) . . . . ? O1 Yb1 N1 Si1 -98.2(6) . . . . ? N2 Yb1 N1 Si1 170.7(8) . . . . ? N5 Yb1 N1 Si1 3.5(7) . . . . ? N6 Yb1 N1 Si1 60.1(7) . . . . ? N4 Yb1 N1 Si1 150.7(5) . . . . ? C1 Yb1 N1 Si1 170.2(11) . . . . ? C45 Yb1 N1 Si1 31.2(7) . . . . ? O1 Yb1 N2 C1 -109.1(6) . . . . ? N5 Yb1 N2 C1 26.4(9) . . . . ? N1 Yb1 N2 C1 -0.5(5) . . . . ? N6 Yb1 N2 C1 78.3(6) . . . . ? N4 Yb1 N2 C1 164.2(6) . . . . ? C45 Yb1 N2 C1 56.5(7) . . . . ? O1 Yb1 N2 C3 69.1(11) . . . . ? N5 Yb1 N2 C3 -155.5(9) . . . . ? N1 Yb1 N2 C3 177.7(12) . . . . ? N6 Yb1 N2 C3 -103.5(10) . . . . ? N4 Yb1 N2 C3 -17.6(10) . . . . ? C1 Yb1 N2 C3 178.2(14) . . . . ? C45 Yb1 N2 C3 -125.3(10) . . . . ? C23 Si2 N3 H3 -131(8) . . . . ? C22 Si2 N3 H3 -13(8) . . . . ? C21 Si2 N3 H3 107(8) . . . . ? C23 Si2 N3 C2 42.5(11) . . . . ? C22 Si2 N3 C2 160.7(10) . . . . ? C21 Si2 N3 C2 -79.2(11) . . . . ? O1 Yb1 N4 C2 119.9(8) . . . . ? N2 Yb1 N4 C2 -136.7(8) . . . . ? N5 Yb1 N4 C2 20.2(9) . . . . ? N1 Yb1 N4 C2 -119.6(8) . . . . ? N6 Yb1 N4 C2 -28.9(8) . . . . ? C1 Yb1 N4 C2 -129.2(8) . . . . ? C45 Yb1 N4 C2 -9.5(9) . . . . ? O1 Yb1 N4 C5 -65.7(6) . . . . ? N2 Yb1 N4 C5 37.6(6) . . . . ? N5 Yb1 N4 C5 -165.5(5) . . . . ? N1 Yb1 N4 C5 54.7(7) . . . . ? N6 Yb1 N4 C5 145.5(6) . . . . ? C1 Yb1 N4 C5 45.2(6) . . . . ? C45 Yb1 N4 C5 164.8(6) . . . . ? O1 Yb1 N5 C45 -169.2(6) . . . . ? N2 Yb1 N5 C45 54.5(8) . . . . ? N1 Yb1 N5 C45 76.9(6) . . . . ? N6 Yb1 N5 C45 -9.4(5) . . . . ? N4 Yb1 N5 C45 -74.0(6) . . . . ? C1 Yb1 N5 C45 69.2(6) . . . . ? O1 Yb1 N5 C39 -10.1(10) . . . . ? N2 Yb1 N5 C39 -146.4(9) . . . . ? N1 Yb1 N5 C39 -124.0(9) . . . . ? N6 Yb1 N5 C39 149.7(10) . . . . ? N4 Yb1 N5 C39 85.1(10) . . . . ? C1 Yb1 N5 C39 -131.7(9) . . . . ? C45 Yb1 N5 C39 159.1(13) . . . . ? O1 Yb1 N6 C45 50.7(8) . . . . ? N2 Yb1 N6 C45 -143.4(5) . . . . ? N5 Yb1 N6 C45 9.3(5) . . . . ? N1 Yb1 N6 C45 -88.1(6) . . . . ? N4 Yb1 N6 C45 140.5(6) . . . . ? C1 Yb1 N6 C45 -115.4(6) . . . . ? O1 Yb1 N6 C46 -167.0(7) . . . . ? N2 Yb1 N6 C46 -1.1(9) . . . . ? N5 Yb1 N6 C46 151.7(9) . . . . ? N1 Yb1 N6 C46 54.3(8) . . . . ? N4 Yb1 N6 C46 -77.2(8) . . . . ? C1 Yb1 N6 C46 26.9(8) . . . . ? C45 Yb1 N6 C46 142.3(11) . . . . ? C3 N2 C1 N1 -177.8(8) . . . . ? Yb1 N2 C1 N1 0.8(9) . . . . ? C3 N2 C1 C6 4.9(14) . . . . ? Yb1 N2 C1 C6 -176.5(8) . . . . ? C3 N2 C1 Yb1 -178.7(10) . . . . ? Si1 N1 C1 N2 -172.8(7) . . . . ? Yb1 N1 C1 N2 -0.8(8) . . . . ? Si1 N1 C1 C6 4.5(14) . . . . ? Yb1 N1 C1 C6 176.5(8) . . . . ? Si1 N1 C1 Yb1 -172.0(9) . . . . ? O1 Yb1 C1 N2 79.2(6) . . . . ? N5 Yb1 C1 N2 -164.8(5) . . . . ? N1 Yb1 C1 N2 179.1(9) . . . . ? N6 Yb1 C1 N2 -108.4(6) . . . . ? N4 Yb1 C1 N2 -15.8(6) . . . . ? C45 Yb1 C1 N2 -136.2(6) . . . . ? O1 Yb1 C1 N1 -99.9(6) . . . . ? N2 Yb1 C1 N1 -179.1(9) . . . . ? N5 Yb1 C1 N1 16.1(7) . . . . ? N6 Yb1 C1 N1 72.4(6) . . . . ? N4 Yb1 C1 N1 165.1(5) . . . . ? C45 Yb1 C1 N1 44.6(6) . . . . ? O1 Yb1 C1 C6 139(11) . . . . ? N2 Yb1 C1 C6 60(11) . . . . ? N5 Yb1 C1 C6 -105(11) . . . . ? N1 Yb1 C1 C6 -121(11) . . . . ? N6 Yb1 C1 C6 -48(11) . . . . ? N4 Yb1 C1 C6 44(11) . . . . ? C45 Yb1 C1 C6 -76(11) . . . . ? C5 N4 C2 N3 -175.8(8) . . . . ? Yb1 N4 C2 N3 -1.8(13) . . . . ? C5 N4 C2 C12 3.5(13) . . . . ? Yb1 N4 C2 C12 177.5(7) . . . . ? H3 N3 C2 N4 11(7) . . . . ? Si2 N3 C2 N4 -163.1(7) . . . . ? H3 N3 C2 C12 -168(7) . . . . ? Si2 N3 C2 C12 17.6(14) . . . . ? C1 N2 C3 C4 -159.0(8) . . . . ? Yb1 N2 C3 C4 23.1(14) . . . . ? N2 C3 C4 C5 -45.5(11) . . . . ? C2 N4 C5 C4 95.3(10) . . . . ? Yb1 N4 C5 C4 -79.9(8) . . . . ? C3 C4 C5 N4 85.5(10) . . . . ? N2 C1 C6 C7 90.5(12) . . . . ? N1 C1 C6 C7 -86.6(12) . . . . ? Yb1 C1 C6 C7 32(12) . . . . ? N2 C1 C6 C11 -90.8(12) . . . . ? N1 C1 C6 C11 92.2(12) . . . . ? Yb1 C1 C6 C11 -149(11) . . . . ? C11 C6 C7 C8 -2.8(15) . . . . ? C1 C6 C7 C8 175.9(9) . . . . ? C6 C7 C8 C9 0.3(16) . . . . ? C7 C8 C9 C10 2.1(17) . . . . ? C8 C9 C10 C11 -1.7(17) . . . . ? C9 C10 C11 C6 -0.9(17) . . . . ? C7 C6 C11 C10 3.2(16) . . . . ? C1 C6 C11 C10 -175.6(9) . . . . ? N4 C2 C12 C17 -100.9(12) . . . . ? N3 C2 C12 C17 78.4(13) . . . . ? N4 C2 C12 C13 74.1(14) . . . . ? N3 C2 C12 C13 -106.6(12) . . . . ? C17 C12 C13 C14 -0.7(17) . . . . ? C2 C12 C13 C14 -175.8(10) . . . . ? C12 C13 C14 C15 0.9(18) . . . . ? C13 C14 C15 C16 -1.1(19) . . . . ? C14 C15 C16 C17 1(2) . . . . ? C13 C12 C17 C16 0.8(18) . . . . ? C2 C12 C17 C16 175.9(11) . . . . ? C15 C16 C17 C12 -1(2) . . . . ? Yb1 O1 C24 C25 92(5) . . . . ? Yb1 O1 C24 C29 -89(5) . . . . ? O1 C24 C25 C26 -179.3(9) . . . . ? C29 C24 C25 C26 2.2(14) . . . . ? O1 C24 C25 C30 6.5(15) . . . . ? C29 C24 C25 C30 -172.0(9) . . . . ? C24 C25 C26 C27 -0.9(16) . . . . ? C30 C25 C26 C27 173.9(10) . . . . ? C25 C26 C27 C28 -1.1(16) . . . . ? C25 C26 C27 C34 179.3(10) . . . . ? C26 C27 C28 C29 1.9(15) . . . . ? C34 C27 C28 C29 -178.5(9) . . . . ? C27 C28 C29 C24 -0.6(14) . . . . ? C27 C28 C29 C35 -178.9(9) . . . . ? O1 C24 C29 C28 180.0(8) . . . . ? C25 C24 C29 C28 -1.5(14) . . . . ? O1 C24 C29 C35 -1.8(14) . . . . ? C25 C24 C29 C35 176.7(8) . . . . ? C26 C25 C30 C31 14.2(14) . . . . ? C24 C25 C30 C31 -171.4(10) . . . . ? C26 C25 C30 C33 136.5(10) . . . . ? C24 C25 C30 C33 -49.1(15) . . . . ? C26 C25 C30 C32 -103.1(11) . . . . ? C24 C25 C30 C32 71.3(12) . . . . ? C28 C29 C35 C38 118.9(9) . . . . ? C24 C29 C35 C38 -59.3(12) . . . . ? C28 C29 C35 C37 -117.8(9) . . . . ? C24 C29 C35 C37 64.0(11) . . . . ? C28 C29 C35 C36 -0.3(12) . . . . ? C24 C29 C35 C36 -178.5(9) . . . . ? C45 N5 C39 C40 36.8(14) . . . . ? Yb1 N5 C39 C40 -118.1(10) . . . . ? C45 N5 C39 C44 -152.9(9) . . . . ? Yb1 N5 C39 C44 52.2(13) . . . . ? N5 C39 C40 C41 172.1(10) . . . . ? C44 C39 C40 C41 1.8(15) . . . . ? C39 C40 C41 C42 -1.3(18) . . . . ? C40 C41 C42 C43 0(2) . . . . ? C41 C42 C43 C44 1(2) . . . . ? C42 C43 C44 C39 -0.7(18) . . . . ? N5 C39 C44 C43 -171.7(10) . . . . ? C40 C39 C44 C43 -0.8(15) . . . . ? C39 N5 C45 N6 -148.4(8) . . . . ? Yb1 N5 C45 N6 15.2(8) . . . . ? C39 N5 C45 N7 34.8(15) . . . . ? Yb1 N5 C45 N7 -161.6(9) . . . . ? C39 N5 C45 Yb1 -163.6(10) . . . . ? C46 N6 C45 N5 -165.7(8) . . . . ? Yb1 N6 C45 N5 -14.8(8) . . . . ? C46 N6 C45 N7 11.3(14) . . . . ? Yb1 N6 C45 N7 162.1(8) . . . . ? C46 N6 C45 Yb1 -150.8(9) . . . . ? C49 N7 C45 N5 18.5(16) . . . . ? C49 N7 C45 N6 -158.0(9) . . . . ? C49 N7 C45 Yb1 -71(3) . . . . ? O1 Yb1 C45 N5 13.3(7) . . . . ? N2 Yb1 C45 N5 -149.3(5) . . . . ? N1 Yb1 C45 N5 -104.6(6) . . . . ? N6 Yb1 C45 N5 163.5(9) . . . . ? N4 Yb1 C45 N5 120.2(6) . . . . ? C1 Yb1 C45 N5 -124.4(6) . . . . ? O1 Yb1 C45 N6 -150.3(5) . . . . ? N2 Yb1 C45 N6 47.2(7) . . . . ? N5 Yb1 C45 N6 -163.5(9) . . . . ? N1 Yb1 C45 N6 91.9(6) . . . . ? N4 Yb1 C45 N6 -43.4(6) . . . . ? C1 Yb1 C45 N6 72.1(6) . . . . ? O1 Yb1 C45 N7 114(3) . . . . ? N2 Yb1 C45 N7 -49(3) . . . . ? N5 Yb1 C45 N7 101(3) . . . . ? N1 Yb1 C45 N7 -4(3) . . . . ? N6 Yb1 C45 N7 -96(3) . . . . ? N4 Yb1 C45 N7 -139(3) . . . . ? C1 Yb1 C45 N7 -24(3) . . . . ? C45 N6 C46 C47 152.6(9) . . . . ? Yb1 N6 C46 C47 17.8(12) . . . . ? C45 N6 C46 C48 -85.6(10) . . . . ? Yb1 N6 C46 C48 139.7(7) . . . . ? C45 N7 C49 C50 -129.4(11) . . . . ? C45 N7 C49 C51 107.5(11) . . . . ? C55 O2 C52 C53 -8(2) . . . . ? O2 C52 C53 C54 -6(3) . . . . ? C52 C53 C54 C55 17(2) . . . . ? C52 O2 C55 C54 17.5(19) . . . . ? C53 C54 C55 O2 -21(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.644 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.132 data_complex9 _database_code_depnum_ccdc_archive 'CCDC 915743' #TrackingRef '915743.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H77 Cl N7 O Si2 Yb, C4 H8 O' _chemical_formula_sum 'C55 H85 Cl N7 O2 Si2 Yb' _chemical_formula_weight 1140.97 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' Yb Yb -0.3850 5.5486 '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' Cl Cl 0.1484 0.1585 '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' _symmetry_Int_Tables_number 14 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 18.079(2) _cell_length_b 18.777(2) _cell_length_c 18.448(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.725(3) _cell_angle_gamma 90.00 _cell_volume 5895.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 25797 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.6 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2380 _exptl_absorpt_coefficient_mu 1.716 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.341 _exptl_absorpt_correction_T_max 0.847 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29491 _diffrn_reflns_av_R_equivalents 0.0817 _diffrn_reflns_av_unetI/netI 0.0985 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10935 _reflns_number_gt 9306 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.Their N3-H3,N7- H7A,and C53-C54 distances were constrained. ; _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^)+(0.0470P)^2^+5.3400P] 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 10935 _refine_ls_number_parameters 612 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0705 _refine_ls_wR_factor_ref 0.1588 _refine_ls_wR_factor_gt 0.1494 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.173 _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 Yb1 Yb 0.835053(17) 0.150698(15) 0.699084(16) 0.02941(12) Uani 1 1 d . . . Cl1 Cl 0.46974(16) 0.32475(15) 0.41807(18) 0.0889(9) Uani 1 1 d . . . Si1 Si 0.97380(13) 0.19105(12) 0.57930(13) 0.0441(5) Uani 1 1 d . . . Si2 Si 0.63174(13) -0.03730(12) 0.72364(12) 0.0434(5) Uani 1 1 d . . . O1 O 0.7862(3) 0.2446(2) 0.7232(2) 0.0334(11) Uani 1 1 d . . . O2 O 0.7155(5) 0.8658(4) 0.4869(4) 0.085(2) Uiso 1 1 d . . . N1 N 0.9486(3) 0.1703(3) 0.6601(3) 0.0357(14) Uani 1 1 d . . . N2 N 0.9616(3) 0.1428(3) 0.7819(3) 0.0388(15) Uani 1 1 d . . . N3 N 0.7133(4) 0.0190(3) 0.7467(3) 0.0365(14) Uani 1 1 d D . . H3 H 0.733(4) 0.031(4) 0.712(3) 0.07(3) Uiso 1 1 d D . . N4 N 0.8176(3) 0.0911(3) 0.8109(3) 0.0322(13) Uani 1 1 d . . . N5 N 0.7428(3) 0.1409(3) 0.5748(3) 0.0301(13) Uani 1 1 d . . . N6 N 0.7985(3) 0.0406(3) 0.6344(3) 0.0297(12) Uani 1 1 d . . . N7 N 0.7225(4) 0.0315(3) 0.5024(3) 0.0343(14) Uani 1 1 d D . . H7A H 0.727(4) -0.0145(8) 0.507(4) 0.04(2) Uiso 1 1 d D . . C1 C 0.9967(4) 0.1622(3) 0.7328(4) 0.0328(16) Uani 1 1 d . . . C2 C 0.7672(4) 0.0431(4) 0.8127(4) 0.0317(15) Uani 1 1 d . . . C3 C 1.0074(5) 0.1301(5) 0.8634(5) 0.053(2) Uani 1 1 d . . . H3A H 1.0214 0.1756 0.8907 0.064 Uiso 1 1 calc R . . H3B H 1.0560 0.1046 0.8677 0.064 Uiso 1 1 calc R . . C4 C 0.9576(5) 0.0858(4) 0.8990(4) 0.048(2) Uani 1 1 d . . . H4A H 0.9531 0.0374 0.8782 0.058 Uiso 1 1 calc R . . H4B H 0.9850 0.0827 0.9547 0.058 Uiso 1 1 calc R . . C5 C 0.8768(5) 0.1145(4) 0.8851(4) 0.049(2) Uani 1 1 d . . . H5A H 0.8591 0.0995 0.9274 0.058 Uiso 1 1 calc R . . H5B H 0.8792 0.1667 0.8857 0.058 Uiso 1 1 calc R . . C6 C 1.0831(4) 0.1746(4) 0.7587(4) 0.0399(18) Uani 1 1 d . . . C7 C 1.1333(5) 0.1313(4) 0.7363(5) 0.050(2) Uani 1 1 d . . . H7 H 1.1126 0.0929 0.7030 0.060 Uiso 1 1 calc R . . C8 C 1.2137(6) 0.1435(5) 0.7619(7) 0.068(3) Uani 1 1 d . . . H8 H 1.2473 0.1127 0.7474 0.081 Uiso 1 1 calc R . . C9 C 1.2441(5) 0.2014(6) 0.8090(6) 0.076(3) Uani 1 1 d . . . H9 H 1.2983 0.2111 0.8258 0.092 Uiso 1 1 calc R . . C10 C 1.1939(6) 0.2445(6) 0.8310(6) 0.073(3) Uani 1 1 d . . . H10 H 1.2141 0.2835 0.8637 0.088 Uiso 1 1 calc R . . C11 C 1.1154(5) 0.2313(4) 0.8060(5) 0.051(2) Uani 1 1 d . . . H11 H 1.0822 0.2618 0.8215 0.061 Uiso 1 1 calc R . . C12 C 0.7652(4) 0.0084(4) 0.8855(4) 0.0373(17) Uani 1 1 d . . . C13 C 0.7268(5) 0.0382(5) 0.9309(5) 0.055(2) Uani 1 1 d . . . H13 H 0.7004 0.0818 0.9166 0.066 Uiso 1 1 calc R . . C14 C 0.7266(6) 0.0048(6) 0.9969(5) 0.069(3) Uani 1 1 d . . . H14 H 0.7002 0.0255 1.0275 0.083 Uiso 1 1 calc R . . C15 C 0.7647(6) -0.0584(5) 1.0183(5) 0.066(3) Uani 1 1 d . . . H15 H 0.7639 -0.0812 1.0634 0.079 Uiso 1 1 calc R . . C16 C 0.8039(6) -0.0889(5) 0.9749(5) 0.065(3) Uani 1 1 d . . . H16 H 0.8311 -0.1319 0.9907 0.078 Uiso 1 1 calc R . . C17 C 0.8034(5) -0.0564(4) 0.9078(4) 0.051(2) Uani 1 1 d . . . H17 H 0.8291 -0.0781 0.8770 0.061 Uiso 1 1 calc R . . C18 C 1.0492(5) 0.2629(5) 0.5936(5) 0.065(3) Uani 1 1 d . . . H18A H 1.0351 0.3033 0.6191 0.097 Uiso 1 1 calc R . . H18B H 1.0514 0.2777 0.5440 0.097 Uiso 1 1 calc R . . H18C H 1.1002 0.2449 0.6252 0.097 Uiso 1 1 calc R . . C19 C 0.8821(5) 0.2223(5) 0.5042(4) 0.055(2) Uani 1 1 d . . . H19A H 0.8392 0.1905 0.5023 0.083 Uiso 1 1 calc R . . H19B H 0.8896 0.2227 0.4545 0.083 Uiso 1 1 calc R . . H19C H 0.8698 0.2701 0.5167 0.083 Uiso 1 1 calc R . . C20 C 1.0100(6) 0.1117(5) 0.5391(5) 0.066(3) Uani 1 1 d . . . H20A H 1.0574 0.0935 0.5773 0.099 Uiso 1 1 calc R . . H20B H 1.0214 0.1258 0.4933 0.099 Uiso 1 1 calc R . . H20C H 0.9699 0.0750 0.5258 0.099 Uiso 1 1 calc R . . C21 C 0.6601(6) -0.1314(5) 0.7358(7) 0.084(3) Uani 1 1 d . . . H21A H 0.6930 -0.1423 0.7052 0.127 Uiso 1 1 calc R . . H21B H 0.6134 -0.1609 0.7190 0.127 Uiso 1 1 calc R . . H21C H 0.6891 -0.1408 0.7897 0.127 Uiso 1 1 calc R . . C22 C 0.5817(5) -0.0171(4) 0.6196(4) 0.050(2) Uani 1 1 d . . . H22A H 0.5620 0.0314 0.6141 0.075 Uiso 1 1 calc R . . H22B H 0.5382 -0.0498 0.5983 0.075 Uiso 1 1 calc R . . H22C H 0.6188 -0.0223 0.5923 0.075 Uiso 1 1 calc R . . C23 C 0.5676(5) -0.0163(6) 0.7798(5) 0.076(3) Uani 1 1 d . . . H23A H 0.5963 -0.0234 0.8341 0.114 Uiso 1 1 calc R . . H23B H 0.5221 -0.0475 0.7639 0.114 Uiso 1 1 calc R . . H23C H 0.5505 0.0328 0.7708 0.114 Uiso 1 1 calc R . . C24 C 0.7467(4) 0.3071(4) 0.7151(4) 0.0353(17) Uani 1 1 d . . . C25 C 0.6674(4) 0.3091(4) 0.7153(4) 0.0354(16) Uani 1 1 d . . . C26 C 0.6250(5) 0.3719(4) 0.6905(4) 0.0446(19) Uani 1 1 d . . . H26 H 0.5718 0.3728 0.6864 0.054 Uiso 1 1 calc R . . C27 C 0.6574(5) 0.4327(4) 0.6715(4) 0.0427(19) Uani 1 1 d . . . C28 C 0.7363(5) 0.4320(4) 0.6837(4) 0.0397(18) Uani 1 1 d . . . H28 H 0.7603 0.4743 0.6757 0.048 Uiso 1 1 calc R . . C29 C 0.7828(4) 0.3718(4) 0.7072(4) 0.0386(17) Uani 1 1 d . . . C30 C 0.6302(4) 0.2468(4) 0.7437(4) 0.0425(18) Uani 1 1 d . . . C31 C 0.5516(5) 0.2677(5) 0.7530(5) 0.060(2) Uani 1 1 d . . . H31A H 0.5607 0.3036 0.7928 0.090 Uiso 1 1 calc R . . H31B H 0.5279 0.2260 0.7672 0.090 Uiso 1 1 calc R . . H31C H 0.5165 0.2866 0.7046 0.090 Uiso 1 1 calc R . . C32 C 0.6852(5) 0.2241(4) 0.8257(4) 0.052(2) Uani 1 1 d . . . H32A H 0.7348 0.2071 0.8227 0.077 Uiso 1 1 calc R . . H32B H 0.6603 0.1864 0.8451 0.077 Uiso 1 1 calc R . . H32C H 0.6946 0.2647 0.8602 0.077 Uiso 1 1 calc R . . C33 C 0.6139(5) 0.1832(4) 0.6881(5) 0.054(2) Uani 1 1 d . . . H33A H 0.5780 0.1977 0.6381 0.080 Uiso 1 1 calc R . . H33B H 0.5905 0.1448 0.7082 0.080 Uiso 1 1 calc R . . H33C H 0.6628 0.1670 0.6829 0.080 Uiso 1 1 calc R . . C34 C 0.6071(5) 0.4984(5) 0.6415(5) 0.060(2) Uani 1 1 d . . . H34A H 0.5793 0.5108 0.6764 0.090 Uiso 1 1 calc R . . H34B H 0.5695 0.4884 0.5908 0.090 Uiso 1 1 calc R . . H34C H 0.6405 0.5378 0.6380 0.090 Uiso 1 1 calc R . . C35 C 0.8711(4) 0.3779(4) 0.7217(5) 0.046(2) Uani 1 1 d . . . C36 C 0.8992(6) 0.4550(5) 0.7308(7) 0.076(3) Uani 1 1 d . . . H36A H 0.8815 0.4786 0.7688 0.114 Uiso 1 1 calc R . . H36B H 0.8778 0.4794 0.6818 0.114 Uiso 1 1 calc R . . H36C H 0.9561 0.4561 0.7475 0.114 Uiso 1 1 calc R . . C37 C 0.8908(5) 0.3454(5) 0.6534(6) 0.062(3) Uani 1 1 d . . . H37A H 0.8625 0.3709 0.6065 0.092 Uiso 1 1 calc R . . H37B H 0.8755 0.2956 0.6476 0.092 Uiso 1 1 calc R . . H37C H 0.9469 0.3492 0.6631 0.092 Uiso 1 1 calc R . . C38 C 0.9192(5) 0.3395(4) 0.7967(5) 0.056(2) Uani 1 1 d . . . H38A H 0.9746 0.3493 0.8080 0.083 Uiso 1 1 calc R . . H38B H 0.9101 0.2886 0.7906 0.083 Uiso 1 1 calc R . . H38C H 0.9031 0.3566 0.8388 0.083 Uiso 1 1 calc R . . C39 C 0.6774(4) 0.1802(4) 0.5324(4) 0.0327(16) Uani 1 1 d . . . C40 C 0.6032(4) 0.1519(4) 0.4940(4) 0.0370(17) Uani 1 1 d . . . H40 H 0.5960 0.1023 0.4916 0.044 Uiso 1 1 calc R . . C41 C 0.5398(4) 0.1967(4) 0.4591(4) 0.046(2) Uani 1 1 d . . . H41 H 0.4898 0.1773 0.4333 0.055 Uiso 1 1 calc R . . C42 C 0.5502(5) 0.2689(4) 0.4624(5) 0.048(2) Uani 1 1 d . . . C43 C 0.6221(5) 0.2985(4) 0.4999(4) 0.0454(19) Uani 1 1 d . . . H43 H 0.6284 0.3482 0.5026 0.054 Uiso 1 1 calc R . . C44 C 0.6851(4) 0.2543(4) 0.5335(4) 0.0371(17) Uani 1 1 d . . . H44 H 0.7348 0.2746 0.5580 0.045 Uiso 1 1 calc R . . C45 C 0.7534(4) 0.0704(4) 0.5683(4) 0.0318(15) Uani 1 1 d . . . C46 C 0.8326(4) -0.0309(4) 0.6355(4) 0.0380(17) Uani 1 1 d . . . H46 H 0.7903 -0.0645 0.6078 0.046 Uiso 1 1 calc R . . C47 C 0.8694(5) -0.0555(4) 0.7181(4) 0.0428(18) Uani 1 1 d . . . H47A H 0.9081 -0.0209 0.7467 0.064 Uiso 1 1 calc R . . H47B H 0.8947 -0.1012 0.7191 0.064 Uiso 1 1 calc R . . H47C H 0.8289 -0.0601 0.7414 0.064 Uiso 1 1 calc R . . C48 C 0.8950(5) -0.0309(5) 0.5972(5) 0.063(3) Uani 1 1 d . . . H48A H 0.8706 -0.0212 0.5427 0.095 Uiso 1 1 calc R . . H48B H 0.9205 -0.0770 0.6042 0.095 Uiso 1 1 calc R . . H48C H 0.9337 0.0057 0.6204 0.095 Uiso 1 1 calc R . . C49 C 0.7082(4) 0.0588(4) 0.4238(4) 0.0396(17) Uani 1 1 d . . . H49 H 0.6959 0.1102 0.4228 0.048 Uiso 1 1 calc R . . C50 C 0.6395(5) 0.0209(5) 0.3680(5) 0.070(3) Uani 1 1 d . . . H50A H 0.6491 -0.0300 0.3714 0.105 Uiso 1 1 calc R . . H50B H 0.6322 0.0371 0.3161 0.105 Uiso 1 1 calc R . . H50C H 0.5925 0.0312 0.3805 0.105 Uiso 1 1 calc R . . C51 C 0.7804(5) 0.0492(5) 0.3999(4) 0.056(2) Uani 1 1 d . . . H51A H 0.8252 0.0721 0.4373 0.083 Uiso 1 1 calc R . . H51B H 0.7708 0.0705 0.3496 0.083 Uiso 1 1 calc R . . H51C H 0.7911 -0.0012 0.3974 0.083 Uiso 1 1 calc R . . C52 C 0.7579(10) 0.8258(8) 0.4494(10) 0.140(4) Uiso 1 1 d . . . H52A H 0.8030 0.8023 0.4870 0.168 Uiso 1 1 calc R . . H52B H 0.7769 0.8565 0.4165 0.168 Uiso 1 1 calc R . . C53 C 0.7020(9) 0.7730(8) 0.4031(10) 0.140(4) Uiso 1 1 d D . . H53A H 0.7284 0.7274 0.4032 0.168 Uiso 1 1 calc R . . H53B H 0.6787 0.7894 0.3497 0.168 Uiso 1 1 calc R . . C54 C 0.6409(9) 0.7654(8) 0.4394(9) 0.137(4) Uiso 1 1 d D . . H54A H 0.6532 0.7256 0.4759 0.165 Uiso 1 1 calc R . . H54B H 0.5892 0.7573 0.4004 0.165 Uiso 1 1 calc R . . C55 C 0.6425(9) 0.8348(8) 0.4803(10) 0.137(4) Uiso 1 1 d . . . H55A H 0.5991 0.8655 0.4505 0.165 Uiso 1 1 calc R . . H55B H 0.6383 0.8267 0.5313 0.165 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 0.0288(2) 0.0348(2) 0.02300(18) -0.00146(12) 0.00656(14) -0.00013(12) Cl1 0.0617(17) 0.0770(17) 0.104(2) 0.0100(16) -0.0039(15) 0.0362(14) Si1 0.0465(13) 0.0505(13) 0.0413(12) 0.0063(10) 0.0226(11) 0.0012(10) Si2 0.0395(12) 0.0518(13) 0.0371(12) 0.0035(10) 0.0107(10) -0.0088(10) O1 0.034(3) 0.038(3) 0.025(2) -0.007(2) 0.005(2) 0.001(2) N1 0.037(3) 0.038(3) 0.029(3) 0.000(3) 0.006(3) 0.003(3) N2 0.023(3) 0.052(4) 0.032(3) 0.004(3) -0.004(3) -0.006(3) N3 0.039(4) 0.048(4) 0.023(3) 0.002(3) 0.010(3) -0.006(3) N4 0.040(3) 0.037(3) 0.020(3) -0.002(2) 0.012(3) -0.003(3) N5 0.028(3) 0.035(3) 0.023(3) -0.004(2) 0.002(2) 0.002(2) N6 0.032(3) 0.035(3) 0.022(3) 0.003(2) 0.010(2) 0.001(2) N7 0.043(4) 0.038(4) 0.020(3) -0.002(3) 0.008(3) -0.002(3) C1 0.034(4) 0.031(4) 0.034(4) -0.003(3) 0.013(3) -0.004(3) C2 0.037(4) 0.036(4) 0.025(4) 0.004(3) 0.015(3) 0.001(3) C3 0.030(4) 0.072(6) 0.043(5) 0.005(4) -0.005(4) -0.005(4) C4 0.045(5) 0.061(5) 0.027(4) 0.000(4) -0.003(3) -0.009(4) C5 0.058(6) 0.059(5) 0.028(4) 0.002(4) 0.013(4) -0.021(4) C6 0.036(4) 0.036(4) 0.044(5) 0.013(4) 0.009(4) 0.002(3) C7 0.044(5) 0.041(4) 0.065(6) 0.014(4) 0.019(4) 0.002(4) C8 0.046(6) 0.064(6) 0.100(8) 0.026(6) 0.034(6) 0.011(5) C9 0.031(5) 0.087(8) 0.093(8) 0.029(7) -0.003(5) -0.014(5) C10 0.055(6) 0.080(7) 0.071(7) 0.013(6) 0.004(5) -0.015(5) C11 0.030(4) 0.053(5) 0.062(6) 0.000(4) 0.005(4) 0.001(4) C12 0.049(5) 0.045(4) 0.020(3) 0.002(3) 0.015(3) -0.006(4) C13 0.070(6) 0.061(6) 0.040(5) 0.009(4) 0.029(5) 0.013(4) C14 0.095(8) 0.081(7) 0.046(5) 0.010(5) 0.044(6) 0.004(6) C15 0.093(8) 0.072(7) 0.032(5) 0.017(5) 0.020(5) -0.012(6) C16 0.089(7) 0.065(6) 0.035(5) 0.012(4) 0.013(5) 0.010(5) C17 0.059(6) 0.060(5) 0.038(4) 0.007(4) 0.020(4) 0.004(4) C18 0.069(6) 0.070(6) 0.069(6) 0.019(5) 0.041(5) -0.004(5) C19 0.065(6) 0.074(6) 0.029(4) 0.014(4) 0.018(4) 0.006(5) C20 0.072(7) 0.079(7) 0.060(6) -0.006(5) 0.038(5) 0.011(5) C21 0.082(8) 0.069(6) 0.085(8) 0.014(6) 0.005(6) -0.013(6) C22 0.041(5) 0.063(5) 0.040(5) -0.011(4) 0.004(4) -0.016(4) C23 0.062(6) 0.123(9) 0.057(6) -0.007(6) 0.037(5) -0.030(6) C24 0.040(4) 0.045(4) 0.013(3) -0.004(3) -0.001(3) 0.006(3) C25 0.041(4) 0.042(4) 0.028(4) -0.009(3) 0.018(3) -0.002(3) C26 0.037(4) 0.056(5) 0.042(5) 0.004(4) 0.016(4) 0.010(4) C27 0.048(5) 0.053(5) 0.028(4) 0.007(3) 0.015(4) 0.017(4) C28 0.051(5) 0.039(4) 0.028(4) 0.000(3) 0.012(4) 0.003(3) C29 0.041(4) 0.039(4) 0.033(4) -0.005(3) 0.009(3) 0.002(3) C30 0.034(4) 0.057(5) 0.039(4) -0.002(4) 0.016(4) 0.004(4) C31 0.061(6) 0.065(6) 0.059(6) 0.013(5) 0.028(5) 0.009(5) C32 0.063(6) 0.058(5) 0.038(5) 0.007(4) 0.022(4) 0.004(4) C33 0.058(6) 0.053(5) 0.054(5) -0.011(4) 0.025(5) -0.017(4) C34 0.072(6) 0.059(5) 0.058(6) 0.022(5) 0.032(5) 0.027(5) C35 0.034(4) 0.038(4) 0.063(5) -0.008(4) 0.012(4) -0.001(3) C36 0.058(6) 0.051(5) 0.118(9) -0.007(6) 0.026(6) -0.008(5) C37 0.051(6) 0.065(6) 0.075(7) -0.004(5) 0.030(5) 0.001(4) C38 0.046(5) 0.053(5) 0.056(6) -0.002(4) 0.002(4) 0.007(4) C39 0.034(4) 0.041(4) 0.024(4) 0.000(3) 0.009(3) 0.005(3) C40 0.034(4) 0.044(4) 0.027(4) -0.003(3) 0.002(3) 0.004(3) C41 0.026(4) 0.066(5) 0.034(4) -0.005(4) -0.005(3) -0.001(4) C42 0.051(5) 0.048(5) 0.040(5) 0.008(4) 0.009(4) 0.019(4) C43 0.056(5) 0.041(4) 0.037(4) 0.002(4) 0.013(4) 0.008(4) C44 0.037(4) 0.047(4) 0.026(4) -0.003(3) 0.008(3) -0.002(3) C45 0.030(4) 0.037(4) 0.031(4) -0.003(3) 0.015(3) -0.005(3) C46 0.041(4) 0.035(4) 0.031(4) 0.001(3) 0.002(3) 0.006(3) C47 0.047(5) 0.049(5) 0.033(4) 0.007(4) 0.014(4) 0.012(4) C48 0.066(6) 0.090(7) 0.038(5) 0.011(5) 0.022(4) 0.033(5) C49 0.050(5) 0.046(4) 0.023(4) -0.003(3) 0.013(3) -0.002(4) C50 0.065(6) 0.102(8) 0.032(5) -0.008(5) 0.003(4) -0.015(6) C51 0.067(6) 0.076(6) 0.025(4) -0.002(4) 0.018(4) -0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O1 2.086(4) . ? Yb1 N2 2.287(6) . ? Yb1 N5 2.343(5) . ? Yb1 N6 2.368(5) . ? Yb1 N1 2.423(6) . ? Yb1 N4 2.459(5) . ? Yb1 C1 2.784(7) . ? Yb1 C45 2.805(7) . ? Cl1 C42 1.756(8) . ? Si1 N1 1.743(6) . ? Si1 C19 1.860(8) . ? Si1 C18 1.872(9) . ? Si1 C20 1.878(9) . ? Si2 N3 1.746(6) . ? Si2 C21 1.832(10) . ? Si2 C23 1.840(8) . ? Si2 C22 1.864(8) . ? O1 C24 1.355(8) . ? O2 C52 1.410(16) . ? O2 C55 1.410(15) . ? N1 C1 1.339(9) . ? N2 C1 1.321(9) . ? N2 C3 1.471(9) . ? N3 C2 1.355(9) . ? N3 H3 0.870(10) . ? N4 C2 1.290(8) . ? N4 C5 1.490(9) . ? N5 C45 1.349(8) . ? N5 C39 1.391(8) . ? N6 C45 1.339(8) . ? N6 C46 1.474(8) . ? N7 C45 1.366(8) . ? N7 C49 1.476(8) . ? N7 H7A 0.870(10) . ? C1 C6 1.490(10) . ? C2 C12 1.504(9) . ? C3 C4 1.527(11) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.497(11) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C11 1.376(11) . ? C6 C7 1.382(11) . ? C7 C8 1.387(12) . ? C7 H7 0.9400 . ? C8 C9 1.384(14) . ? C8 H8 0.9400 . ? C9 C10 1.376(14) . ? C9 H9 0.9400 . ? C10 C11 1.359(12) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C13 1.373(10) . ? C12 C17 1.391(10) . ? C13 C14 1.371(11) . ? C13 H13 0.9400 . ? C14 C15 1.361(13) . ? C14 H14 0.9400 . ? C15 C16 1.360(13) . ? C15 H15 0.9400 . ? C16 C17 1.378(11) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C29 1.409(10) . ? C24 C25 1.435(10) . ? C25 C26 1.396(10) . ? C25 C30 1.528(10) . ? C26 C27 1.381(11) . ? C26 H26 0.9400 . ? C27 C28 1.367(10) . ? C27 C34 1.522(10) . ? C28 C29 1.387(10) . ? C28 H28 0.9400 . ? C29 C35 1.531(10) . ? C30 C33 1.538(10) . ? C30 C31 1.539(10) . ? C30 C32 1.562(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 C36 1.525(11) . ? C35 C38 1.541(11) . ? C35 C37 1.548(12) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 C40 1.393(9) . ? C39 C44 1.398(9) . ? C40 C41 1.393(10) . ? C40 H40 0.9400 . ? C41 C42 1.367(11) . ? C41 H41 0.9400 . ? C42 C43 1.367(11) . ? C43 C44 1.376(10) . ? C43 H43 0.9400 . ? C44 H44 0.9400 . ? C46 C47 1.514(9) . ? C46 C48 1.519(11) . ? C46 H46 0.9900 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 C50 1.498(10) . ? C49 C51 1.522(10) . ? C49 H49 0.9900 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C50 H50C 0.9700 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C52 C53 1.467(18) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.480(14) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.501(18) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 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 O1 Yb1 N2 108.2(2) . . ? O1 Yb1 N5 93.58(18) . . ? N2 Yb1 N5 150.4(2) . . ? O1 Yb1 N6 141.19(18) . . ? N2 Yb1 N6 109.1(2) . . ? N5 Yb1 N6 56.80(18) . . ? O1 Yb1 N1 113.41(18) . . ? N2 Yb1 N1 56.7(2) . . ? N5 Yb1 N1 96.68(19) . . ? N6 Yb1 N1 95.97(18) . . ? O1 Yb1 N4 91.26(18) . . ? N2 Yb1 N4 78.0(2) . . ? N5 Yb1 N4 122.30(19) . . ? N6 Yb1 N4 86.11(18) . . ? N1 Yb1 N4 132.85(19) . . ? O1 Yb1 C1 112.06(19) . . ? N2 Yb1 C1 28.1(2) . . ? N5 Yb1 C1 124.9(2) . . ? N6 Yb1 C1 105.89(19) . . ? N1 Yb1 C1 28.74(19) . . ? N4 Yb1 C1 105.7(2) . . ? O1 Yb1 C45 120.00(18) . . ? N2 Yb1 C45 131.1(2) . . ? N5 Yb1 C45 28.61(18) . . ? N6 Yb1 C45 28.42(18) . . ? N1 Yb1 C45 94.53(19) . . ? N4 Yb1 C45 107.31(19) . . ? C1 Yb1 C45 116.21(19) . . ? N1 Si1 C19 106.4(3) . . ? N1 Si1 C18 115.3(4) . . ? C19 Si1 C18 107.5(4) . . ? N1 Si1 C20 112.8(4) . . ? C19 Si1 C20 107.3(4) . . ? C18 Si1 C20 107.0(4) . . ? N3 Si2 C21 112.0(4) . . ? N3 Si2 C23 112.0(4) . . ? C21 Si2 C23 110.0(5) . . ? N3 Si2 C22 101.8(3) . . ? C21 Si2 C22 109.9(5) . . ? C23 Si2 C22 110.9(4) . . ? C24 O1 Yb1 162.4(4) . . ? C52 O2 C55 112.7(11) . . ? C1 N1 Si1 127.9(5) . . ? C1 N1 Yb1 90.8(4) . . ? Si1 N1 Yb1 141.3(3) . . ? C1 N2 C3 120.7(6) . . ? C1 N2 Yb1 97.4(4) . . ? C3 N2 Yb1 141.7(5) . . ? C2 N3 Si2 135.5(5) . . ? C2 N3 H3 103(6) . . ? Si2 N3 H3 121(6) . . ? C2 N4 C5 118.5(6) . . ? C2 N4 Yb1 129.1(4) . . ? C5 N4 Yb1 112.4(4) . . ? C45 N5 C39 126.2(6) . . ? C45 N5 Yb1 95.1(4) . . ? C39 N5 Yb1 134.3(4) . . ? C45 N6 C46 121.1(5) . . ? C45 N6 Yb1 94.2(4) . . ? C46 N6 Yb1 138.0(4) . . ? C45 N7 C49 125.0(6) . . ? C45 N7 H7A 116(5) . . ? C49 N7 H7A 115(5) . . ? N2 C1 N1 114.7(6) . . ? N2 C1 C6 121.2(6) . . ? N1 C1 C6 124.0(6) . . ? N2 C1 Yb1 54.5(4) . . ? N1 C1 Yb1 60.5(4) . . ? C6 C1 Yb1 172.8(5) . . ? N4 C2 N3 120.7(6) . . ? N4 C2 C12 123.8(6) . . ? N3 C2 C12 115.5(6) . . ? N2 C3 C4 108.5(6) . . ? N2 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? N2 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? C5 C4 C3 114.4(7) . . ? C5 C4 H4A 108.7 . . ? C3 C4 H4A 108.7 . . ? C5 C4 H4B 108.7 . . ? C3 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? N4 C5 C4 114.1(7) . . ? N4 C5 H5A 108.7 . . ? C4 C5 H5A 108.7 . . ? N4 C5 H5B 108.7 . . ? C4 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C11 C6 C7 117.7(7) . . ? C11 C6 C1 119.9(7) . . ? C7 C6 C1 122.4(7) . . ? C6 C7 C8 121.3(9) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C7 119.4(9) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 119.0(9) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C11 C10 C9 120.7(10) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C6 121.8(9) . . ? C10 C11 H11 119.1 . . ? C6 C11 H11 119.1 . . ? C13 C12 C17 118.6(7) . . ? C13 C12 C2 122.5(7) . . ? C17 C12 C2 118.9(6) . . ? C14 C13 C12 120.5(8) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C15 C14 C13 120.3(9) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 120.6(8) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 119.7(8) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C12 120.3(8) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O1 C24 C29 120.9(7) . . ? O1 C24 C25 120.8(7) . . ? C29 C24 C25 118.3(7) . . ? C26 C25 C24 117.4(7) . . ? C26 C25 C30 120.1(7) . . ? C24 C25 C30 122.4(6) . . ? C27 C26 C25 123.2(7) . . ? C27 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? C28 C27 C26 117.3(7) . . ? C28 C27 C34 122.0(8) . . ? C26 C27 C34 120.6(7) . . ? C27 C28 C29 123.2(7) . . ? C27 C28 H28 118.4 . . ? C29 C28 H28 118.4 . . ? C28 C29 C24 118.8(7) . . ? C28 C29 C35 118.6(7) . . ? C24 C29 C35 122.5(7) . . ? C25 C30 C33 111.9(6) . . ? C25 C30 C31 111.9(6) . . ? C33 C30 C31 107.1(7) . . ? C25 C30 C32 109.4(6) . . ? C33 C30 C32 110.5(7) . . ? C31 C30 C32 105.8(6) . . ? 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 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C27 C34 H34A 109.5 . . ? C27 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C27 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C29 112.3(6) . . ? C36 C35 C38 106.2(7) . . ? C29 C35 C38 111.2(7) . . ? C36 C35 C37 107.7(7) . . ? C29 C35 C37 110.0(7) . . ? C38 C35 C37 109.4(7) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N5 C39 C40 125.0(7) . . ? N5 C39 C44 117.3(6) . . ? C40 C39 C44 117.5(6) . . ? C41 C40 C39 120.4(7) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C42 C41 C40 119.9(7) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C43 121.2(7) . . ? C41 C42 Cl1 119.4(6) . . ? C43 C42 Cl1 119.3(6) . . ? C42 C43 C44 119.0(7) . . ? C42 C43 H43 120.5 . . ? C44 C43 H43 120.5 . . ? C43 C44 C39 122.0(7) . . ? C43 C44 H44 119.0 . . ? C39 C44 H44 119.0 . . ? N6 C45 N5 113.0(6) . . ? N6 C45 N7 121.9(6) . . ? N5 C45 N7 125.2(6) . . ? N6 C45 Yb1 57.3(3) . . ? N5 C45 Yb1 56.3(3) . . ? N7 C45 Yb1 172.5(5) . . ? N6 C46 C47 109.4(6) . . ? N6 C46 C48 111.5(6) . . ? C47 C46 C48 109.0(6) . . ? N6 C46 H46 109.0 . . ? C47 C46 H46 109.0 . . ? C48 C46 H46 109.0 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N7 C49 C50 109.8(6) . . ? N7 C49 C51 111.1(6) . . ? C50 C49 C51 109.8(7) . . ? N7 C49 H49 108.7 . . ? C50 C49 H49 108.7 . . ? C51 C49 H49 108.7 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O2 C52 C53 105.4(13) . . ? O2 C52 H52A 110.7 . . ? C53 C52 H52A 110.7 . . ? O2 C52 H52B 110.7 . . ? C53 C52 H52B 110.7 . . ? H52A C52 H52B 108.8 . . ? C52 C53 C54 105.9(14) . . ? C52 C53 H53A 110.6 . . ? C54 C53 H53A 110.6 . . ? C52 C53 H53B 110.6 . . ? C54 C53 H53B 110.6 . . ? H53A C53 H53B 108.7 . . ? C53 C54 C55 104.7(13) . . ? C53 C54 H54A 110.8 . . ? C55 C54 H54A 110.8 . . ? C53 C54 H54B 110.8 . . ? C55 C54 H54B 110.8 . . ? H54A C54 H54B 108.9 . . ? O2 C55 C54 105.1(13) . . ? O2 C55 H55A 110.7 . . ? C54 C55 H55A 110.7 . . ? O2 C55 H55B 110.7 . . ? C54 C55 H55B 110.7 . . ? H55A C55 H55B 108.8 . . ? 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 N2 Yb1 O1 C24 134.9(15) . . . . ? N5 Yb1 O1 C24 -24.8(15) . . . . ? N6 Yb1 O1 C24 -61.9(16) . . . . ? N1 Yb1 O1 C24 74.0(15) . . . . ? N4 Yb1 O1 C24 -147.3(15) . . . . ? C1 Yb1 O1 C24 105.2(15) . . . . ? C45 Yb1 O1 C24 -36.4(15) . . . . ? C19 Si1 N1 C1 -162.7(6) . . . . ? C18 Si1 N1 C1 -43.5(7) . . . . ? C20 Si1 N1 C1 79.9(7) . . . . ? C19 Si1 N1 Yb1 13.6(6) . . . . ? C18 Si1 N1 Yb1 132.7(5) . . . . ? C20 Si1 N1 Yb1 -103.8(6) . . . . ? O1 Yb1 N1 C1 93.5(4) . . . . ? N2 Yb1 N1 C1 -3.5(4) . . . . ? N5 Yb1 N1 C1 -169.6(4) . . . . ? N6 Yb1 N1 C1 -112.5(4) . . . . ? N4 Yb1 N1 C1 -22.2(5) . . . . ? C45 Yb1 N1 C1 -141.0(4) . . . . ? O1 Yb1 N1 Si1 -83.6(5) . . . . ? N2 Yb1 N1 Si1 179.4(6) . . . . ? N5 Yb1 N1 Si1 13.3(5) . . . . ? N6 Yb1 N1 Si1 70.5(5) . . . . ? N4 Yb1 N1 Si1 160.7(4) . . . . ? C1 Yb1 N1 Si1 -177.1(8) . . . . ? C45 Yb1 N1 Si1 42.0(5) . . . . ? O1 Yb1 N2 C1 -102.9(4) . . . . ? N5 Yb1 N2 C1 32.6(7) . . . . ? N6 Yb1 N2 C1 88.2(4) . . . . ? N1 Yb1 N2 C1 3.6(4) . . . . ? N4 Yb1 N2 C1 169.7(5) . . . . ? C45 Yb1 N2 C1 67.1(5) . . . . ? O1 Yb1 N2 C3 70.8(8) . . . . ? N5 Yb1 N2 C3 -153.7(7) . . . . ? N6 Yb1 N2 C3 -98.1(8) . . . . ? N1 Yb1 N2 C3 177.4(9) . . . . ? N4 Yb1 N2 C3 -16.5(8) . . . . ? C1 Yb1 N2 C3 173.7(11) . . . . ? C45 Yb1 N2 C3 -119.2(8) . . . . ? C21 Si2 N3 C2 -77.4(9) . . . . ? C23 Si2 N3 C2 46.6(9) . . . . ? C22 Si2 N3 C2 165.2(7) . . . . ? O1 Yb1 N4 C2 106.2(6) . . . . ? N2 Yb1 N4 C2 -145.4(6) . . . . ? N5 Yb1 N4 C2 11.2(7) . . . . ? N6 Yb1 N4 C2 -35.0(6) . . . . ? N1 Yb1 N4 C2 -129.5(6) . . . . ? C1 Yb1 N4 C2 -140.4(6) . . . . ? C45 Yb1 N4 C2 -15.8(6) . . . . ? O1 Yb1 N4 C5 -75.7(5) . . . . ? N2 Yb1 N4 C5 32.7(5) . . . . ? N5 Yb1 N4 C5 -170.7(5) . . . . ? N6 Yb1 N4 C5 143.1(5) . . . . ? N1 Yb1 N4 C5 48.6(6) . . . . ? C1 Yb1 N4 C5 37.7(5) . . . . ? C45 Yb1 N4 C5 162.3(5) . . . . ? O1 Yb1 N5 C45 -158.7(4) . . . . ? N2 Yb1 N5 C45 63.2(6) . . . . ? N6 Yb1 N5 C45 -5.6(4) . . . . ? N1 Yb1 N5 C45 87.2(4) . . . . ? N4 Yb1 N5 C45 -64.9(4) . . . . ? C1 Yb1 N5 C45 81.2(4) . . . . ? O1 Yb1 N5 C39 -2.3(6) . . . . ? N2 Yb1 N5 C39 -140.4(6) . . . . ? N6 Yb1 N5 C39 150.9(7) . . . . ? N1 Yb1 N5 C39 -116.4(6) . . . . ? N4 Yb1 N5 C39 91.5(6) . . . . ? C1 Yb1 N5 C39 -122.4(6) . . . . ? C45 Yb1 N5 C39 156.4(9) . . . . ? O1 Yb1 N6 C45 51.6(5) . . . . ? N2 Yb1 N6 C45 -145.3(4) . . . . ? N5 Yb1 N6 C45 5.6(4) . . . . ? N1 Yb1 N6 C45 -88.5(4) . . . . ? N4 Yb1 N6 C45 138.8(4) . . . . ? C1 Yb1 N6 C45 -116.0(4) . . . . ? O1 Yb1 N6 C46 -159.4(6) . . . . ? N2 Yb1 N6 C46 3.7(7) . . . . ? N5 Yb1 N6 C46 154.6(7) . . . . ? N1 Yb1 N6 C46 60.5(6) . . . . ? N4 Yb1 N6 C46 -72.2(6) . . . . ? C1 Yb1 N6 C46 33.0(7) . . . . ? C45 Yb1 N6 C46 149.0(8) . . . . ? C3 N2 C1 N1 178.5(6) . . . . ? Yb1 N2 C1 N1 -6.0(6) . . . . ? C3 N2 C1 C6 -2.5(10) . . . . ? Yb1 N2 C1 C6 173.0(5) . . . . ? C3 N2 C1 Yb1 -175.5(8) . . . . ? Si1 N1 C1 N2 -176.7(5) . . . . ? Yb1 N1 C1 N2 5.6(6) . . . . ? Si1 N1 C1 C6 4.4(10) . . . . ? Yb1 N1 C1 C6 -173.3(6) . . . . ? Si1 N1 C1 Yb1 177.7(6) . . . . ? O1 Yb1 C1 N2 87.5(4) . . . . ? N5 Yb1 C1 N2 -161.1(4) . . . . ? N6 Yb1 C1 N2 -100.8(4) . . . . ? N1 Yb1 C1 N2 -173.7(7) . . . . ? N4 Yb1 C1 N2 -10.4(5) . . . . ? C45 Yb1 C1 N2 -129.3(4) . . . . ? O1 Yb1 C1 N1 -98.8(4) . . . . ? N2 Yb1 C1 N1 173.7(7) . . . . ? N5 Yb1 C1 N1 12.6(5) . . . . ? N6 Yb1 C1 N1 72.9(4) . . . . ? N4 Yb1 C1 N1 163.3(4) . . . . ? C45 Yb1 C1 N1 44.4(4) . . . . ? O1 Yb1 C1 C6 31(4) . . . . ? N2 Yb1 C1 C6 -56(4) . . . . ? N5 Yb1 C1 C6 143(4) . . . . ? N6 Yb1 C1 C6 -157(4) . . . . ? N1 Yb1 C1 C6 130(4) . . . . ? N4 Yb1 C1 C6 -67(4) . . . . ? C45 Yb1 C1 C6 174(4) . . . . ? C5 N4 C2 N3 -178.6(7) . . . . ? Yb1 N4 C2 N3 -0.5(10) . . . . ? C5 N4 C2 C12 -0.9(10) . . . . ? Yb1 N4 C2 C12 177.1(5) . . . . ? Si2 N3 C2 N4 -173.1(6) . . . . ? Si2 N3 C2 C12 9.1(11) . . . . ? C1 N2 C3 C4 -161.3(7) . . . . ? Yb1 N2 C3 C4 26.0(12) . . . . ? N2 C3 C4 C5 -50.8(9) . . . . ? C2 N4 C5 C4 105.0(8) . . . . ? Yb1 N4 C5 C4 -73.4(7) . . . . ? C3 C4 C5 N4 86.0(8) . . . . ? N2 C1 C6 C11 -67.6(10) . . . . ? N1 C1 C6 C11 111.3(9) . . . . ? Yb1 C1 C6 C11 -15(4) . . . . ? N2 C1 C6 C7 113.1(8) . . . . ? N1 C1 C6 C7 -68.0(10) . . . . ? Yb1 C1 C6 C7 165(4) . . . . ? C11 C6 C7 C8 1.5(12) . . . . ? C1 C6 C7 C8 -179.2(8) . . . . ? C6 C7 C8 C9 -2.0(14) . . . . ? C7 C8 C9 C10 1.7(15) . . . . ? C8 C9 C10 C11 -1.0(15) . . . . ? C9 C10 C11 C6 0.5(15) . . . . ? C7 C6 C11 C10 -0.8(13) . . . . ? C1 C6 C11 C10 179.9(8) . . . . ? N4 C2 C12 C13 85.1(10) . . . . ? N3 C2 C12 C13 -97.2(9) . . . . ? N4 C2 C12 C17 -95.1(9) . . . . ? N3 C2 C12 C17 82.7(9) . . . . ? C17 C12 C13 C14 0.3(13) . . . . ? C2 C12 C13 C14 -179.8(8) . . . . ? C12 C13 C14 C15 0.1(15) . . . . ? C13 C14 C15 C16 0.6(16) . . . . ? C14 C15 C16 C17 -1.6(15) . . . . ? C15 C16 C17 C12 2.0(14) . . . . ? C13 C12 C17 C16 -1.3(13) . . . . ? C2 C12 C17 C16 178.8(8) . . . . ? Yb1 O1 C24 C29 -83.9(16) . . . . ? Yb1 O1 C24 C25 96.8(15) . . . . ? O1 C24 C25 C26 -166.6(6) . . . . ? C29 C24 C25 C26 14.1(9) . . . . ? O1 C24 C25 C30 15.5(9) . . . . ? C29 C24 C25 C30 -163.9(6) . . . . ? C24 C25 C26 C27 -4.9(11) . . . . ? C30 C25 C26 C27 173.1(7) . . . . ? C25 C26 C27 C28 -5.1(11) . . . . ? C25 C26 C27 C34 177.3(7) . . . . ? C26 C27 C28 C29 5.9(11) . . . . ? C34 C27 C28 C29 -176.5(7) . . . . ? C27 C28 C29 C24 3.5(11) . . . . ? C27 C28 C29 C35 -177.8(7) . . . . ? O1 C24 C29 C28 167.1(6) . . . . ? C25 C24 C29 C28 -13.5(10) . . . . ? O1 C24 C29 C35 -11.5(10) . . . . ? C25 C24 C29 C35 167.9(7) . . . . ? C26 C25 C30 C33 111.1(8) . . . . ? C24 C25 C30 C33 -71.0(9) . . . . ? C26 C25 C30 C31 -9.2(10) . . . . ? C24 C25 C30 C31 168.7(7) . . . . ? C26 C25 C30 C32 -126.1(7) . . . . ? C24 C25 C30 C32 51.8(8) . . . . ? C28 C29 C35 C36 16.9(11) . . . . ? C24 C29 C35 C36 -164.5(8) . . . . ? C28 C29 C35 C38 135.7(7) . . . . ? C24 C29 C35 C38 -45.7(9) . . . . ? C28 C29 C35 C37 -103.0(8) . . . . ? C24 C29 C35 C37 75.7(9) . . . . ? C45 N5 C39 C40 21.0(11) . . . . ? Yb1 N5 C39 C40 -129.4(6) . . . . ? C45 N5 C39 C44 -164.5(6) . . . . ? Yb1 N5 C39 C44 45.2(9) . . . . ? N5 C39 C40 C41 173.9(7) . . . . ? C44 C39 C40 C41 -0.7(10) . . . . ? C39 C40 C41 C42 0.1(12) . . . . ? C40 C41 C42 C43 -0.4(12) . . . . ? C40 C41 C42 Cl1 179.9(6) . . . . ? C41 C42 C43 C44 1.2(12) . . . . ? Cl1 C42 C43 C44 -179.0(6) . . . . ? C42 C43 C44 C39 -1.8(11) . . . . ? N5 C39 C44 C43 -173.4(7) . . . . ? C40 C39 C44 C43 1.6(10) . . . . ? C46 N6 C45 N5 -165.1(6) . . . . ? Yb1 N6 C45 N5 -8.8(6) . . . . ? C46 N6 C45 N7 14.9(10) . . . . ? Yb1 N6 C45 N7 171.2(6) . . . . ? C46 N6 C45 Yb1 -156.3(7) . . . . ? C39 N5 C45 N6 -150.3(6) . . . . ? Yb1 N5 C45 N6 9.0(6) . . . . ? C39 N5 C45 N7 29.7(11) . . . . ? Yb1 N5 C45 N7 -171.1(6) . . . . ? C39 N5 C45 Yb1 -159.2(7) . . . . ? C49 N7 C45 N6 -147.7(7) . . . . ? C49 N7 C45 N5 32.4(11) . . . . ? C49 N7 C45 Yb1 -66(4) . . . . ? O1 Yb1 C45 N6 -145.4(4) . . . . ? N2 Yb1 C45 N6 45.5(5) . . . . ? N5 Yb1 C45 N6 -170.2(6) . . . . ? N1 Yb1 C45 N6 94.2(4) . . . . ? N4 Yb1 C45 N6 -43.5(4) . . . . ? C1 Yb1 C45 N6 74.4(4) . . . . ? O1 Yb1 C45 N5 24.8(5) . . . . ? N2 Yb1 C45 N5 -144.3(4) . . . . ? N6 Yb1 C45 N5 170.2(6) . . . . ? N1 Yb1 C45 N5 -95.6(4) . . . . ? N4 Yb1 C45 N5 126.7(4) . . . . ? C1 Yb1 C45 N5 -115.4(4) . . . . ? O1 Yb1 C45 N7 128(4) . . . . ? N2 Yb1 C45 N7 -41(4) . . . . ? N5 Yb1 C45 N7 104(4) . . . . ? N6 Yb1 C45 N7 -86(4) . . . . ? N1 Yb1 C45 N7 8(4) . . . . ? N4 Yb1 C45 N7 -130(4) . . . . ? C1 Yb1 C45 N7 -12(4) . . . . ? C45 N6 C46 C47 -171.1(6) . . . . ? Yb1 N6 C46 C47 45.8(9) . . . . ? C45 N6 C46 C48 68.3(8) . . . . ? Yb1 N6 C46 C48 -74.8(8) . . . . ? C45 N7 C49 C50 -149.7(7) . . . . ? C45 N7 C49 C51 88.6(8) . . . . ? C55 O2 C52 C53 11.4(17) . . . . ? O2 C52 C53 C54 -22.7(18) . . . . ? C52 C53 C54 C55 25.2(18) . . . . ? C52 O2 C55 C54 4.4(17) . . . . ? C53 C54 C55 O2 -18.3(17) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.906 _refine_diff_density_min -1.601 _refine_diff_density_rms 0.118 data_complex2 _database_code_depnum_ccdc_archive 'CCDC 915744' #TrackingRef '915744.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H61 N4 O3 Si2 Y' _chemical_formula_sum 'C39 H61 N4 O3 Si2 Y' _chemical_formula_weight 779.01 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' Y Y -2.7962 3.5667 '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' _symmetry_Int_Tables_number 14 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 24.6655(11) _cell_length_b 8.6830(3) _cell_length_c 20.0629(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.124(4) _cell_angle_gamma 90.00 _cell_volume 4127.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6621 _cell_measurement_theta_min 3.4110 _cell_measurement_theta_max 28.8760 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 1.510 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.68864 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3818 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28966 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_unetI/netI 0.0415 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7688 _reflns_number_gt 5965 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their C4-C5,C12-C17', C14'-C15',C15'-C16',C12-C13,C12-C17' and C12-C13' distances were constrained. ; _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^)+(0.0548P)^2^+8.6684P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7688 _refine_ls_number_parameters 431 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1292 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.254520(13) 0.74785(4) 0.276063(16) 0.01363(11) Uani 1 1 d . B . Si1 Si 0.09909(4) 0.89727(11) 0.27490(5) 0.0172(2) Uani 1 1 d . . . Si2 Si 0.40062(4) 0.92048(13) 0.25904(6) 0.0266(3) Uani 1 1 d . . . O1 O 0.22626(9) 0.5970(3) 0.19210(11) 0.0167(5) Uani 1 1 d . . . O2 O 0.26924(13) 1.0111(3) 0.32114(13) 0.0322(7) Uani 1 1 d . . . O3 O 0.23023(10) 0.9474(3) 0.18771(11) 0.0169(5) Uani 1 1 d . . . N1 N 0.16232(14) 0.7989(5) 0.30196(17) 0.0351(5) Uani 1 1 d . . . N2 N 0.22794(14) 0.6414(4) 0.36875(17) 0.0351(5) Uani 1 1 d . . . N3 N 0.35567(12) 0.7966(4) 0.28478(15) 0.0221(7) Uani 1 1 d . B . N4 N 0.33067(14) 0.5928(4) 0.34091(18) 0.0368(9) Uani 1 1 d . B . C1 C 0.17730(17) 0.7022(6) 0.3561(2) 0.0351(5) Uani 1 1 d . . . C2 C 0.37048(16) 0.6940(5) 0.3367(2) 0.0325(10) Uani 1 1 d . . . C3 C 0.2475(2) 0.5262(7) 0.4244(3) 0.0614(10) Uani 1 1 d . . . H3A H 0.2327 0.5524 0.4640 0.074 Uiso 1 1 calc R . . H3B H 0.2329 0.4233 0.4070 0.074 Uiso 1 1 calc R . . C4 C 0.3098(2) 0.5218(7) 0.4478(3) 0.0614(10) Uani 1 1 d D B . H4A H 0.3232 0.6245 0.4668 0.074 Uiso 1 1 calc R . . H4B H 0.3210 0.4474 0.4866 0.074 Uiso 1 1 calc R . . C5 C 0.3400(2) 0.4814(7) 0.3974(3) 0.0614(10) Uani 1 1 d D . . H5A H 0.3274 0.3785 0.3780 0.074 Uiso 1 1 calc R B . H5B H 0.3808 0.4754 0.4212 0.074 Uiso 1 1 calc R . . C6 C 0.13920(14) 0.6623(4) 0.40032(18) 0.0217(8) Uani 1 1 d . . . C7 C 0.13349(14) 0.7647(4) 0.45119(18) 0.0218(8) Uani 1 1 d . . . H7 H 0.1537 0.8591 0.4580 0.026 Uiso 1 1 calc R . . C8 C 0.09801(15) 0.7285(5) 0.49202(19) 0.0258(9) Uani 1 1 d . . . H8 H 0.0940 0.7985 0.5267 0.031 Uiso 1 1 calc R . . C9 C 0.06867(15) 0.5914(5) 0.48226(19) 0.0280(9) Uani 1 1 d . . . H9 H 0.0441 0.5676 0.5098 0.034 Uiso 1 1 calc R . . C10 C 0.07500(16) 0.4889(5) 0.43257(19) 0.0288(9) Uani 1 1 d . . . H10 H 0.0548 0.3943 0.4259 0.035 Uiso 1 1 calc R . . C11 C 0.11057(17) 0.5234(5) 0.39247(19) 0.0273(9) Uani 1 1 d . . . H11 H 0.1155 0.4512 0.3591 0.033 Uiso 1 1 calc R . . C12 C 0.42774(15) 0.6891(5) 0.3862(2) 0.0324(10) Uani 1 1 d D A . C13 C 0.4369(4) 0.7975(14) 0.4416(6) 0.0437(9) Uani 0.50 1 d PD A 1 H13A H 0.4069 0.8646 0.4434 0.052 Uiso 0.50 1 calc PR A 1 C13' C 0.4521(4) 0.7968(15) 0.4333(6) 0.0437(9) Uani 0.50 1 d PD A 2 H13B H 0.4315 0.8847 0.4406 0.052 Uiso 0.50 1 calc PR A 2 C14 C 0.4881(4) 0.8092(13) 0.4935(5) 0.0437(9) Uani 0.50 1 d P A 1 H14A H 0.4928 0.8813 0.5303 0.052 Uiso 0.50 1 calc PR A 1 C14' C 0.5083(4) 0.7762(13) 0.4711(5) 0.0437(9) Uani 0.50 1 d PD A 2 H14B H 0.5259 0.8479 0.5062 0.052 Uiso 0.50 1 calc PR A 2 C15 C 0.5321(4) 0.7114(14) 0.4896(5) 0.0437(9) Uani 0.50 1 d P A 1 H15A H 0.5681 0.7223 0.5222 0.052 Uiso 0.50 1 calc PR A 1 C15' C 0.5380(4) 0.6540(13) 0.4579(6) 0.0437(9) Uani 0.50 1 d PD A 2 H15B H 0.5769 0.6463 0.4821 0.052 Uiso 0.50 1 calc PR A 2 C16 C 0.5240(4) 0.5963(15) 0.4376(5) 0.0437(9) Uani 0.50 1 d P A 1 H16A H 0.5534 0.5263 0.4368 0.052 Uiso 0.50 1 calc PR A 1 C16' C 0.5145(4) 0.5417(13) 0.4113(5) 0.0437(9) Uani 0.50 1 d PD A 2 H16B H 0.5359 0.4551 0.4045 0.052 Uiso 0.50 1 calc PR A 2 C17 C 0.4726(4) 0.5884(14) 0.3884(6) 0.0437(9) Uani 0.50 1 d PD A 1 H17A H 0.4672 0.5103 0.3540 0.052 Uiso 0.50 1 calc PR A 1 C17' C 0.4584(4) 0.5582(13) 0.3742(6) 0.0437(9) Uani 0.50 1 d PD A 2 H17B H 0.4405 0.4827 0.3411 0.052 Uiso 0.50 1 calc PR A 2 C18 C 0.09882(16) 1.0727(4) 0.32942(19) 0.0246(8) Uani 1 1 d . . . H18A H 0.0982 1.0411 0.3761 0.037 Uiso 1 1 calc R . . H18B H 0.0653 1.1349 0.3082 0.037 Uiso 1 1 calc R . . H18C H 0.1328 1.1337 0.3325 0.037 Uiso 1 1 calc R . . C19 C 0.03486(15) 0.7827(5) 0.2741(2) 0.0310(9) Uani 1 1 d . . . H19A H 0.0361 0.6837 0.2510 0.047 Uiso 1 1 calc R . . H19B H 0.0011 0.8397 0.2488 0.047 Uiso 1 1 calc R . . H19C H 0.0336 0.7646 0.3218 0.047 Uiso 1 1 calc R . . C20 C 0.08960(16) 0.9578(5) 0.18323(19) 0.0282(9) Uani 1 1 d . . . H20A H 0.1224 1.0180 0.1801 0.042 Uiso 1 1 calc R . . H20B H 0.0555 1.0210 0.1677 0.042 Uiso 1 1 calc R . . H20C H 0.0859 0.8664 0.1537 0.042 Uiso 1 1 calc R . . C21 C 0.4761(6) 0.8536(18) 0.2722(8) 0.044(3) Uani 0.70 1 d P B 1 H21A H 0.4963 0.8576 0.3217 0.067 Uiso 0.70 1 calc PR B 1 H21B H 0.4948 0.9210 0.2463 0.067 Uiso 0.70 1 calc PR B 1 H21C H 0.4761 0.7476 0.2554 0.067 Uiso 0.70 1 calc PR B 1 C21' C 0.4636(15) 0.812(4) 0.2482(18) 0.048(8) Uani 0.30 1 d P B 2 H21D H 0.4916 0.8010 0.2934 0.072 Uiso 0.30 1 calc PR B 2 H21E H 0.4803 0.8685 0.2165 0.072 Uiso 0.30 1 calc PR B 2 H21F H 0.4517 0.7097 0.2290 0.072 Uiso 0.30 1 calc PR B 2 C22 C 0.4096(2) 1.1057(5) 0.3099(2) 0.0474(13) Uani 1 1 d . B . H22A H 0.3727 1.1537 0.3042 0.071 Uiso 1 1 calc R . . H22B H 0.4339 1.1759 0.2929 0.071 Uiso 1 1 calc R . . H22C H 0.4270 1.0838 0.3592 0.071 Uiso 1 1 calc R . . C23 C 0.3693(2) 0.9650(5) 0.1657(2) 0.0381(11) Uani 1 1 d . B . H23A H 0.3678 0.8709 0.1383 0.057 Uiso 1 1 calc R . . H23B H 0.3925 1.0422 0.1509 0.057 Uiso 1 1 calc R . . H23C H 0.3310 1.0053 0.1587 0.057 Uiso 1 1 calc R . . C24 C 0.21407(14) 0.5026(4) 0.13741(16) 0.0158(7) Uani 1 1 d . . . C25 C 0.15853(15) 0.4448(4) 0.11109(17) 0.0176(7) Uani 1 1 d . . . C26 C 0.14726(16) 0.3449(4) 0.05462(18) 0.0232(8) Uani 1 1 d . . . H26 H 0.1101 0.3062 0.0363 0.028 Uiso 1 1 calc R . . C27 C 0.18896(17) 0.3008(4) 0.02462(18) 0.0254(9) Uani 1 1 d . . . H27 H 0.1806 0.2307 -0.0132 0.030 Uiso 1 1 calc R . . C28 C 0.24278(17) 0.3591(4) 0.05004(18) 0.0247(8) Uani 1 1 d . . . H28 H 0.2712 0.3285 0.0292 0.030 Uiso 1 1 calc R . . C29 C 0.25645(15) 0.4618(4) 0.10559(17) 0.0187(7) Uani 1 1 d . . . C30 C 0.11391(14) 0.4915(4) 0.14567(18) 0.0195(8) Uani 1 1 d . . . H30 H 0.1181 0.6047 0.1548 0.023 Uiso 1 1 calc R . . C31 C 0.12314(16) 0.4113(4) 0.21579(18) 0.0230(8) Uani 1 1 d . . . H31A H 0.1186 0.2999 0.2087 0.035 Uiso 1 1 calc R . . H31B H 0.0954 0.4493 0.2387 0.035 Uiso 1 1 calc R . . H31C H 0.1613 0.4334 0.2450 0.035 Uiso 1 1 calc R . . C32 C 0.05284(16) 0.4632(5) 0.1023(2) 0.0319(9) Uani 1 1 d . . . H32A H 0.0470 0.5093 0.0563 0.048 Uiso 1 1 calc R . . H32B H 0.0268 0.5102 0.1255 0.048 Uiso 1 1 calc R . . H32C H 0.0457 0.3522 0.0975 0.048 Uiso 1 1 calc R . . C33 C 0.31565(15) 0.5250(4) 0.13427(18) 0.0206(8) Uani 1 1 d . . . H33 H 0.3122 0.6285 0.1546 0.025 Uiso 1 1 calc R . . C34 C 0.34740(19) 0.5472(6) 0.0795(2) 0.0413(11) Uani 1 1 d . . . H34A H 0.3549 0.4466 0.0618 0.062 Uiso 1 1 calc R . . H34B H 0.3832 0.6000 0.1004 0.062 Uiso 1 1 calc R . . H34C H 0.3244 0.6094 0.0412 0.062 Uiso 1 1 calc R . . C35 C 0.35042(16) 0.4232(5) 0.1930(2) 0.0281(9) Uani 1 1 d . . . H35A H 0.3311 0.4145 0.2294 0.042 Uiso 1 1 calc R . . H35B H 0.3877 0.4694 0.2124 0.042 Uiso 1 1 calc R . . H35C H 0.3547 0.3206 0.1748 0.042 Uiso 1 1 calc R . . C36 C 0.24065(19) 1.1294(5) 0.2788(2) 0.0345(10) Uani 1 1 d . . . H36A H 0.2592 1.2287 0.2954 0.041 Uiso 1 1 calc R . . H36B H 0.2015 1.1345 0.2823 0.041 Uiso 1 1 calc R . . C37 C 0.23943(18) 1.1073(4) 0.20530(19) 0.0265(9) Uani 1 1 d . . . H37A H 0.2088 1.1700 0.1751 0.032 Uiso 1 1 calc R . . H37B H 0.2757 1.1413 0.1980 0.032 Uiso 1 1 calc R . . C38 C 0.27517(19) 1.0336(5) 0.39320(19) 0.0336(10) Uani 1 1 d . . . H38A H 0.2949 1.1310 0.4083 0.050 Uiso 1 1 calc R . . H38B H 0.2970 0.9484 0.4197 0.050 Uiso 1 1 calc R . . H38C H 0.2377 1.0369 0.4012 0.050 Uiso 1 1 calc R . . C39 C 0.21284(16) 0.9231(4) 0.11370(17) 0.0245(8) Uani 1 1 d . . . H39A H 0.1765 0.9740 0.0937 0.037 Uiso 1 1 calc R . . H39B H 0.2090 0.8124 0.1040 0.037 Uiso 1 1 calc R . . H39C H 0.2412 0.9664 0.0932 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.01748(17) 0.01195(17) 0.01061(16) 0.00067(14) 0.00250(12) -0.00077(13) Si1 0.0148(4) 0.0173(5) 0.0183(5) 0.0010(4) 0.0027(4) 0.0033(4) Si2 0.0192(5) 0.0254(6) 0.0380(6) 0.0095(5) 0.0126(5) 0.0007(4) O1 0.0200(12) 0.0147(12) 0.0143(12) -0.0010(10) 0.0032(10) -0.0020(10) O2 0.0607(19) 0.0202(14) 0.0147(13) -0.0026(11) 0.0089(13) -0.0016(13) O3 0.0236(12) 0.0126(12) 0.0126(12) 0.0023(10) 0.0017(10) -0.0002(10) N1 0.0289(11) 0.0529(14) 0.0287(11) 0.0222(11) 0.0167(9) 0.0210(10) N2 0.0289(11) 0.0529(14) 0.0287(11) 0.0222(11) 0.0167(9) 0.0210(10) N3 0.0190(15) 0.0260(16) 0.0199(16) 0.0035(14) 0.0028(13) -0.0042(13) N4 0.0296(18) 0.039(2) 0.039(2) 0.0115(18) 0.0061(16) 0.0035(16) C1 0.0289(11) 0.0529(14) 0.0287(11) 0.0222(11) 0.0167(9) 0.0210(10) C2 0.0176(19) 0.050(3) 0.028(2) 0.013(2) 0.0025(17) -0.0054(18) C3 0.0482(17) 0.088(2) 0.0559(19) 0.0476(19) 0.0272(15) 0.0341(17) C4 0.0482(17) 0.088(2) 0.0559(19) 0.0476(19) 0.0272(15) 0.0341(17) C5 0.0482(17) 0.088(2) 0.0559(19) 0.0476(19) 0.0272(15) 0.0341(17) C6 0.0195(18) 0.030(2) 0.0153(18) 0.0073(16) 0.0054(15) 0.0102(16) C7 0.0153(16) 0.027(2) 0.0220(18) 0.0050(17) 0.0030(14) 0.0012(15) C8 0.0225(19) 0.037(2) 0.0190(18) -0.0033(17) 0.0072(15) 0.0036(17) C9 0.0190(18) 0.048(3) 0.0187(19) 0.0059(19) 0.0077(15) -0.0010(18) C10 0.029(2) 0.028(2) 0.024(2) 0.0067(18) -0.0012(17) -0.0065(17) C11 0.037(2) 0.026(2) 0.0175(19) 0.0023(17) 0.0058(17) 0.0110(18) C12 0.0162(18) 0.053(3) 0.027(2) 0.017(2) 0.0035(16) -0.0026(18) C13 0.0226(19) 0.066(2) 0.038(2) 0.0118(17) 0.0006(14) -0.0028(16) C13' 0.0226(19) 0.066(2) 0.038(2) 0.0118(17) 0.0006(14) -0.0028(16) C14 0.0226(19) 0.066(2) 0.038(2) 0.0118(17) 0.0006(14) -0.0028(16) C14' 0.0226(19) 0.066(2) 0.038(2) 0.0118(17) 0.0006(14) -0.0028(16) C15 0.0226(19) 0.066(2) 0.038(2) 0.0118(17) 0.0006(14) -0.0028(16) C15' 0.0226(19) 0.066(2) 0.038(2) 0.0118(17) 0.0006(14) -0.0028(16) C16 0.0226(19) 0.066(2) 0.038(2) 0.0118(17) 0.0006(14) -0.0028(16) C16' 0.0226(19) 0.066(2) 0.038(2) 0.0118(17) 0.0006(14) -0.0028(16) C17 0.0226(19) 0.066(2) 0.038(2) 0.0118(17) 0.0006(14) -0.0028(16) C17' 0.0226(19) 0.066(2) 0.038(2) 0.0118(17) 0.0006(14) -0.0028(16) C18 0.028(2) 0.0195(19) 0.0235(19) 0.0034(16) 0.0018(16) 0.0038(16) C19 0.0175(18) 0.025(2) 0.046(3) 0.0017(19) -0.0001(18) -0.0007(16) C20 0.030(2) 0.032(2) 0.0193(19) 0.0021(17) 0.0018(16) 0.0119(18) C21 0.019(6) 0.051(8) 0.066(9) 0.022(6) 0.018(6) 0.003(5) C21' 0.030(17) 0.06(2) 0.06(2) 0.032(15) 0.023(15) 0.002(12) C22 0.051(3) 0.035(3) 0.043(3) 0.009(2) -0.009(2) -0.017(2) C23 0.058(3) 0.028(2) 0.036(2) 0.002(2) 0.026(2) -0.003(2) C24 0.0241(18) 0.0125(16) 0.0098(16) 0.0028(14) 0.0028(14) -0.0001(14) C25 0.0263(18) 0.0119(17) 0.0118(16) 0.0056(14) 0.0008(14) 0.0011(14) C26 0.034(2) 0.0157(18) 0.0149(18) -0.0009(15) -0.0026(16) -0.0043(16) C27 0.046(2) 0.0158(18) 0.0128(17) -0.0030(15) 0.0060(17) -0.0025(17) C28 0.042(2) 0.0192(19) 0.0158(18) 0.0002(16) 0.0127(17) 0.0026(17) C29 0.0298(19) 0.0117(17) 0.0148(17) 0.0047(14) 0.0065(15) -0.0003(15) C30 0.0192(18) 0.0153(17) 0.0204(18) 0.0005(15) -0.0005(15) -0.0025(14) C31 0.0278(19) 0.0205(19) 0.0210(18) -0.0007(16) 0.0072(16) -0.0004(16) C32 0.025(2) 0.037(2) 0.030(2) 0.0052(19) 0.0005(17) -0.0061(18) C33 0.0276(19) 0.0180(18) 0.0200(18) -0.0012(15) 0.0127(15) -0.0009(15) C34 0.044(3) 0.055(3) 0.033(2) -0.005(2) 0.025(2) -0.012(2) C35 0.0238(19) 0.026(2) 0.034(2) -0.0008(18) 0.0077(17) 0.0003(16) C36 0.047(3) 0.018(2) 0.029(2) -0.0035(18) -0.0061(19) 0.0016(18) C37 0.044(2) 0.0140(18) 0.0238(19) 0.0013(16) 0.0130(17) -0.0013(17) C38 0.053(3) 0.029(2) 0.018(2) -0.0088(18) 0.0077(19) -0.006(2) C39 0.035(2) 0.0226(19) 0.0139(17) 0.0015(16) 0.0034(16) -0.0008(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O1 2.095(2) . ? Y1 N2 2.328(3) . ? Y1 N4 2.382(3) . ? Y1 O3 2.432(2) . ? Y1 O2 2.448(3) . ? Y1 N3 2.488(3) . ? Y1 N1 2.509(3) . ? Y1 C2 2.819(4) . ? Y1 C1 2.839(4) . ? Si1 N1 1.728(3) . ? Si1 C20 1.864(4) . ? Si1 C19 1.867(4) . ? Si1 C18 1.876(4) . ? Si2 N3 1.724(3) . ? Si2 C23 1.857(4) . ? Si2 C21' 1.88(4) . ? Si2 C22 1.885(5) . ? Si2 C21 1.897(17) . ? O1 C24 1.335(4) . ? O2 C36 1.393(5) . ? O2 C38 1.426(4) . ? O3 C37 1.435(4) . ? O3 C39 1.442(4) . ? N1 C1 1.341(5) . ? N2 C1 1.314(5) . ? N2 C3 1.477(5) . ? N3 C2 1.342(5) . ? N4 C2 1.338(5) . ? N4 C5 1.459(6) . ? C1 C6 1.501(5) . ? C2 C12 1.484(5) . ? C3 C4 1.477(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.454(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C11 1.384(6) . ? C6 C7 1.390(5) . ? C7 C8 1.391(5) . ? C7 H7 0.9500 . ? C8 C9 1.379(6) . ? C8 H8 0.9500 . ? C9 C10 1.377(6) . ? C9 H9 0.9500 . ? C10 C11 1.378(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13' 1.347(12) . ? C12 C17 1.400(11) . ? C12 C17' 1.422(12) . ? C12 C13 1.427(12) . ? C13 C14 1.401(13) . ? C13 H13A 0.9500 . ? C13' C14' 1.396(13) . ? C13' H13B 0.9500 . ? C14 C15 1.398(16) . ? C14 H14A 0.9500 . ? C14' C15' 1.357(13) . ? C14' H14B 0.9500 . ? C15 C16 1.418(16) . ? C15 H15A 0.9500 . ? C15' C16' 1.364(12) . ? C15' H15B 0.9500 . ? C16 C17 1.377(13) . ? C16 H16A 0.9500 . ? C16' C17' 1.385(12) . ? C16' H16B 0.9500 . ? C17 H17A 0.9500 . ? C17' H17B 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21' H21D 0.9800 . ? C21' H21E 0.9800 . ? C21' H21F 0.9800 . ? 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 1.413(5) . ? C24 C25 1.416(5) . ? C25 C26 1.392(5) . ? C25 C30 1.510(5) . ? C26 C27 1.382(5) . ? C26 H26 0.9500 . ? C27 C28 1.379(6) . ? C27 H27 0.9500 . ? C28 C29 1.394(5) . ? C28 H28 0.9500 . ? C29 C33 1.516(5) . ? C30 C31 1.529(5) . ? C30 C32 1.536(5) . ? 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 C34 1.529(5) . ? C33 C35 1.531(5) . ? 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 . ? C36 C37 1.479(5) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 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 O1 Y1 N2 106.83(12) . . ? O1 Y1 N4 96.98(11) . . ? N2 Y1 N4 72.16(11) . . ? O1 Y1 O3 84.26(8) . . ? N2 Y1 O3 142.95(10) . . ? N4 Y1 O3 142.94(10) . . ? O1 Y1 O2 149.68(9) . . ? N2 Y1 O2 96.97(12) . . ? N4 Y1 O2 108.20(11) . . ? O3 Y1 O2 65.49(8) . . ? O1 Y1 N3 105.43(10) . . ? N2 Y1 N3 120.71(11) . . ? N4 Y1 N3 55.57(11) . . ? O3 Y1 N3 88.24(9) . . ? O2 Y1 N3 76.84(10) . . ? O1 Y1 N1 99.14(11) . . ? N2 Y1 N1 55.40(11) . . ? N4 Y1 N1 127.54(11) . . ? O3 Y1 N1 88.34(9) . . ? O2 Y1 N1 78.95(12) . . ? N3 Y1 N1 154.71(12) . . ? O1 Y1 C2 108.33(12) . . ? N2 Y1 C2 93.81(11) . . ? N4 Y1 C2 28.24(12) . . ? O3 Y1 C2 116.60(10) . . ? O2 Y1 C2 88.10(12) . . ? N3 Y1 C2 28.42(11) . . ? N1 Y1 C2 144.03(11) . . ? O1 Y1 C1 103.98(12) . . ? N2 Y1 C1 27.23(11) . . ? N4 Y1 C1 99.39(12) . . ? O3 Y1 C1 116.33(10) . . ? O2 Y1 C1 88.60(12) . . ? N3 Y1 C1 143.23(11) . . ? N1 Y1 C1 28.19(11) . . ? C2 Y1 C1 119.50(11) . . ? N1 Si1 C20 107.73(16) . . ? N1 Si1 C19 115.42(18) . . ? C20 Si1 C19 105.52(19) . . ? N1 Si1 C18 111.53(18) . . ? C20 Si1 C18 109.05(18) . . ? C19 Si1 C18 107.31(18) . . ? N3 Si2 C23 108.03(18) . . ? N3 Si2 C21' 110.0(11) . . ? C23 Si2 C21' 96.5(11) . . ? N3 Si2 C22 111.0(2) . . ? C23 Si2 C22 108.8(2) . . ? C21' Si2 C22 120.9(9) . . ? N3 Si2 C21 117.1(5) . . ? C23 Si2 C21 108.8(5) . . ? C21' Si2 C21 18.7(10) . . ? C22 Si2 C21 102.8(4) . . ? C24 O1 Y1 173.4(2) . . ? C36 O2 C38 114.2(3) . . ? C36 O2 Y1 117.7(2) . . ? C38 O2 Y1 117.8(2) . . ? C37 O3 C39 112.1(3) . . ? C37 O3 Y1 121.3(2) . . ? C39 O3 Y1 126.1(2) . . ? C1 N1 Si1 125.8(3) . . ? C1 N1 Y1 89.7(2) . . ? Si1 N1 Y1 144.41(17) . . ? C1 N2 C3 120.8(3) . . ? C1 N2 Y1 98.6(2) . . ? C3 N2 Y1 140.1(3) . . ? C2 N3 Si2 126.0(3) . . ? C2 N3 Y1 89.6(2) . . ? Si2 N3 Y1 143.20(17) . . ? C2 N4 C5 121.6(4) . . ? C2 N4 Y1 94.3(3) . . ? C5 N4 Y1 136.8(3) . . ? N2 C1 N1 116.2(3) . . ? N2 C1 C6 120.7(3) . . ? N1 C1 C6 123.1(3) . . ? N2 C1 Y1 54.16(19) . . ? N1 C1 Y1 62.1(2) . . ? C6 C1 Y1 174.2(3) . . ? N4 C2 N3 116.0(3) . . ? N4 C2 C12 121.2(4) . . ? N3 C2 C12 122.8(3) . . ? N4 C2 Y1 57.4(2) . . ? N3 C2 Y1 61.97(19) . . ? C12 C2 Y1 163.0(3) . . ? C4 C3 N2 110.6(4) . . ? C4 C3 H3A 109.5 . . ? N2 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C5 C4 C3 118.2(5) . . ? C5 C4 H4A 107.8 . . ? C3 C4 H4A 107.8 . . ? C5 C4 H4B 107.8 . . ? C3 C4 H4B 107.8 . . ? H4A C4 H4B 107.1 . . ? C4 C5 N4 112.4(4) . . ? C4 C5 H5A 109.1 . . ? N4 C5 H5A 109.1 . . ? C4 C5 H5B 109.1 . . ? N4 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C11 C6 C7 119.2(3) . . ? C11 C6 C1 121.1(4) . . ? C7 C6 C1 119.6(4) . . ? C6 C7 C8 119.8(4) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 120.2(4) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 120.0(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.0(4) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C6 120.7(4) . . ? C10 C11 H11 119.6 . . ? C6 C11 H11 119.6 . . ? C13' C12 C17 102.5(7) . . ? C13' C12 C17' 121.3(7) . . ? C17 C12 C17' 19.0(6) . . ? C13' C12 C13 18.5(5) . . ? C17 C12 C13 115.8(7) . . ? C17' C12 C13 133.1(7) . . ? C13' C12 C2 127.3(6) . . ? C17 C12 C2 129.4(6) . . ? C17' C12 C2 111.2(5) . . ? C13 C12 C2 114.7(5) . . ? C14 C13 C12 122.8(9) . . ? C14 C13 H13A 118.6 . . ? C12 C13 H13A 118.6 . . ? C12 C13' C14' 118.3(10) . . ? C12 C13' H13B 120.8 . . ? C14' C13' H13B 120.8 . . ? C15 C14 C13 117.9(10) . . ? C15 C14 H14A 121.0 . . ? C13 C14 H14A 121.0 . . ? C15' C14' C13' 120.2(10) . . ? C15' C14' H14B 119.9 . . ? C13' C14' H14B 119.9 . . ? C14 C15 C16 121.1(9) . . ? C14 C15 H15A 119.4 . . ? C16 C15 H15A 119.4 . . ? C14' C15' C16' 122.9(9) . . ? C14' C15' H15B 118.6 . . ? C16' C15' H15B 118.6 . . ? C17 C16 C15 118.5(10) . . ? C17 C16 H16A 120.8 . . ? C15 C16 H16A 120.8 . . ? C15' C16' C17' 117.8(10) . . ? C15' C16' H16B 121.1 . . ? C17' C16' H16B 121.1 . . ? C16 C17 C12 123.6(10) . . ? C16 C17 H17A 118.2 . . ? C12 C17 H17A 118.2 . . ? C16' C17' C12 119.4(9) . . ? C16' C17' H17B 120.3 . . ? C12 C17' H17B 120.3 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? Si2 C21' H21D 109.5 . . ? Si2 C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? Si2 C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O1 C24 C29 120.0(3) . . ? O1 C24 C25 119.8(3) . . ? C29 C24 C25 120.2(3) . . ? C26 C25 C24 118.5(3) . . ? C26 C25 C30 122.3(3) . . ? C24 C25 C30 119.1(3) . . ? C27 C26 C25 121.5(3) . . ? C27 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C28 C27 C26 119.6(3) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 121.6(4) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? C28 C29 C24 118.5(3) . . ? C28 C29 C33 121.9(3) . . ? C24 C29 C33 119.5(3) . . ? C25 C30 C31 111.1(3) . . ? C25 C30 C32 115.0(3) . . ? C31 C30 C32 108.7(3) . . ? C25 C30 H30 107.3 . . ? C31 C30 H30 107.3 . . ? C32 C30 H30 107.3 . . ? 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 . . ? C29 C33 C34 113.9(3) . . ? C29 C33 C35 111.0(3) . . ? C34 C33 C35 109.7(3) . . ? C29 C33 H33 107.3 . . ? C34 C33 H33 107.3 . . ? C35 C33 H33 107.3 . . ? 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 . . ? O2 C36 C37 112.3(3) . . ? O2 C36 H36A 109.1 . . ? C37 C36 H36A 109.1 . . ? O2 C36 H36B 109.1 . . ? C37 C36 H36B 109.1 . . ? H36A C36 H36B 107.9 . . ? O3 C37 C36 109.2(3) . . ? O3 C37 H37A 109.8 . . ? C36 C37 H37A 109.8 . . ? O3 C37 H37B 109.8 . . ? C36 C37 H37B 109.8 . . ? H37A C37 H37B 108.3 . . ? O2 C38 H38A 109.5 . . ? O2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O3 C39 H39A 109.5 . . ? O3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.551 _refine_diff_density_min -1.507 _refine_diff_density_rms 0.084 data_complex1 _database_code_depnum_ccdc_archive 'CCDC 915745' #TrackingRef '915745.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H53 N4 O3 Si2 Y, C7 H8' _chemical_formula_sum 'C42 H61 N4 O3 Si2 Y' _chemical_formula_weight 815.04 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a b' _symmetry_space_group_name_Hall '-P 2bc 2ac' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 8.6929(2) _cell_length_b 52.4298(17) _cell_length_c 19.5627(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8916.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 11494 _cell_measurement_theta_min 2.8109 _cell_measurement_theta_max 29.4473 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 1.401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76524 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3818 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 84018 _diffrn_reflns_av_R_equivalents 0.1233 _diffrn_reflns_av_unetI/netI 0.0687 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -62 _diffrn_reflns_limit_k_max 63 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8290 _reflns_number_gt 6660 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their C36-C37,C40-C41, C41-C36,C37-C38,C36-C42 and C4-C5 distances were constrained. ; _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^)+(0.0182P)^2^+54.5980P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8290 _refine_ls_number_parameters 427 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1209 _refine_ls_R_factor_gt 0.0986 _refine_ls_wR_factor_ref 0.1810 _refine_ls_wR_factor_gt 0.1725 _refine_ls_goodness_of_fit_ref 1.193 _refine_ls_restrained_S_all 1.208 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.27830(6) 0.388254(10) 0.66020(3) 0.02288(16) Uani 1 1 d . . . Si1 Si 0.4183(2) 0.32227(4) 0.74539(11) 0.0390(5) Uani 1 1 d . . . Si2 Si 0.4400(2) 0.45861(3) 0.61255(9) 0.0284(4) Uani 1 1 d . . . O1 O 0.1087(5) 0.40278(9) 0.7264(2) 0.0382(11) Uani 1 1 d . . . O2 O 0.5422(5) 0.37896(9) 0.6247(2) 0.0345(11) Uani 1 1 d . . . O3 O 0.4672(5) 0.39969(8) 0.7437(2) 0.0277(9) Uani 1 1 d . . . N1 N 0.3020(6) 0.34258(9) 0.6983(3) 0.0310(12) Uani 1 1 d . . . N2 N 0.1337(8) 0.35474(10) 0.6171(3) 0.0511(18) Uani 1 1 d . . . N3 N 0.3468(6) 0.42987(9) 0.6029(2) 0.0265(11) Uani 1 1 d . . . N4 N 0.2167(8) 0.39916(11) 0.5487(3) 0.0475(13) Uani 1 1 d . . . C1 C 0.1994(8) 0.33597(12) 0.6511(4) 0.0344(15) Uani 1 1 d . . . C2 C 0.2590(10) 0.42286(13) 0.5502(4) 0.0475(13) Uani 1 1 d . . . C3 C 0.0269(12) 0.34995(17) 0.5606(4) 0.0716(17) Uani 1 1 d . . . H3A H -0.0732 0.3443 0.5794 0.086 Uiso 1 1 calc R . . H3B H 0.0678 0.3359 0.5319 0.086 Uiso 1 1 calc R . . C4 C 0.0021(11) 0.37264(17) 0.5174(5) 0.0716(17) Uani 1 1 d D . . H4A H -0.0544 0.3668 0.4763 0.086 Uiso 1 1 calc R . . H4B H -0.0685 0.3840 0.5428 0.086 Uiso 1 1 calc R . . C5 C 0.1271(11) 0.38826(18) 0.4935(4) 0.0716(17) Uani 1 1 d D . . H5A H 0.0851 0.4022 0.4651 0.086 Uiso 1 1 calc R . . H5B H 0.1954 0.3778 0.4643 0.086 Uiso 1 1 calc R . . C6 C 0.1551(8) 0.30883(12) 0.6365(4) 0.0372(16) Uani 1 1 d . . . C7 C 0.2376(11) 0.29401(15) 0.5918(5) 0.061(2) Uani 1 1 d . . . H7 H 0.3239 0.3011 0.5689 0.073 Uiso 1 1 calc R . . C8 C 0.1966(12) 0.26868(17) 0.5793(6) 0.077(3) Uani 1 1 d . . . H8 H 0.2540 0.2586 0.5480 0.093 Uiso 1 1 calc R . . C9 C 0.0729(14) 0.25849(17) 0.6127(7) 0.090(4) Uani 1 1 d . . . H9 H 0.0455 0.2412 0.6055 0.108 Uiso 1 1 calc R . . C10 C -0.0109(11) 0.27324(16) 0.6563(6) 0.075(3) Uani 1 1 d . . . H10 H -0.0974 0.2661 0.6789 0.091 Uiso 1 1 calc R . . C11 C 0.0278(9) 0.29849(14) 0.6682(5) 0.053(2) Uani 1 1 d . . . H11 H -0.0330 0.3086 0.6980 0.064 Uiso 1 1 calc R . . C12 C 0.2074(7) 0.44135(11) 0.4962(3) 0.0272(14) Uani 1 1 d . . . C13 C 0.2983(7) 0.44682(12) 0.4400(3) 0.0299(14) Uani 1 1 d . . . H13 H 0.3946 0.4385 0.4344 0.036 Uiso 1 1 calc R . . C14 C 0.2493(9) 0.46438(13) 0.3919(3) 0.0396(17) Uani 1 1 d . . . H14 H 0.3135 0.4683 0.3541 0.048 Uiso 1 1 calc R . . C15 C 0.1091(10) 0.47619(13) 0.3983(4) 0.047(2) Uani 1 1 d . . . H15 H 0.0770 0.4884 0.3653 0.056 Uiso 1 1 calc R . . C16 C 0.0149(9) 0.47029(15) 0.4528(4) 0.0474(19) Uani 1 1 d . . . H16 H -0.0829 0.4782 0.4572 0.057 Uiso 1 1 calc R . . C17 C 0.0633(8) 0.45281(14) 0.5011(3) 0.0398(17) Uani 1 1 d . . . H17 H -0.0026 0.4486 0.5382 0.048 Uiso 1 1 calc R . . C18 C 0.3410(11) 0.28940(15) 0.7642(5) 0.068(3) Uani 1 1 d . . . H18A H 0.2417 0.2909 0.7876 0.101 Uiso 1 1 calc R . . H18B H 0.4138 0.2802 0.7934 0.101 Uiso 1 1 calc R . . H18C H 0.3272 0.2801 0.7212 0.101 Uiso 1 1 calc R . . C19 C 0.4553(11) 0.33723(16) 0.8300(4) 0.060(2) Uani 1 1 d . . . H19A H 0.5128 0.3531 0.8236 0.091 Uiso 1 1 calc R . . H19B H 0.5156 0.3255 0.8584 0.091 Uiso 1 1 calc R . . H19C H 0.3572 0.3409 0.8526 0.091 Uiso 1 1 calc R . . C20 C 0.6081(9) 0.31772(17) 0.7011(5) 0.066(3) Uani 1 1 d . . . H20A H 0.5920 0.3086 0.6580 0.099 Uiso 1 1 calc R . . H20B H 0.6771 0.3078 0.7306 0.099 Uiso 1 1 calc R . . H20C H 0.6543 0.3344 0.6916 0.099 Uiso 1 1 calc R . . C21 C 0.3261(9) 0.48763(13) 0.5912(4) 0.0474(19) Uani 1 1 d . . . H21A H 0.3018 0.4876 0.5423 0.071 Uiso 1 1 calc R . . H21B H 0.3862 0.5029 0.6024 0.071 Uiso 1 1 calc R . . H21C H 0.2304 0.4876 0.6177 0.071 Uiso 1 1 calc R . . C22 C 0.6205(8) 0.46016(14) 0.5601(4) 0.0462(18) Uani 1 1 d . . . H22A H 0.6887 0.4461 0.5728 0.069 Uiso 1 1 calc R . . H22B H 0.6728 0.4764 0.5685 0.069 Uiso 1 1 calc R . . H22C H 0.5943 0.4588 0.5115 0.069 Uiso 1 1 calc R . . C23 C 0.4998(9) 0.46215(14) 0.7038(4) 0.0450(19) Uani 1 1 d . . . H23A H 0.4086 0.4617 0.7332 0.068 Uiso 1 1 calc R . . H23B H 0.5532 0.4785 0.7098 0.068 Uiso 1 1 calc R . . H23C H 0.5691 0.4481 0.7162 0.068 Uiso 1 1 calc R . . C24 C 0.0123(7) 0.41039(13) 0.7748(3) 0.0326(15) Uani 1 1 d . . . C25 C -0.0330(8) 0.39392(15) 0.8256(3) 0.0413(18) Uani 1 1 d . . . C26 C -0.1344(9) 0.4021(2) 0.8763(4) 0.060(2) Uani 1 1 d . . . H26 H -0.1655 0.3906 0.9112 0.072 Uiso 1 1 calc R . . C27 C -0.1892(9) 0.4264(2) 0.8762(4) 0.063(3) Uani 1 1 d . . . H27 H -0.2566 0.4320 0.9114 0.076 Uiso 1 1 calc R . . C28 C -0.1468(8) 0.44294(17) 0.8250(4) 0.053(2) Uani 1 1 d . . . H28 H -0.1873 0.4598 0.8248 0.064 Uiso 1 1 calc R . . C29 C -0.0457(8) 0.43555(14) 0.7733(4) 0.0414(18) Uani 1 1 d . . . C30 C 0.0222(11) 0.36622(19) 0.8259(5) 0.082(3) Uani 1 1 d . . . H30A H -0.0066 0.3580 0.7827 0.124 Uiso 1 1 calc R . . H30B H -0.0257 0.3571 0.8641 0.124 Uiso 1 1 calc R . . H30C H 0.1343 0.3658 0.8311 0.124 Uiso 1 1 calc R . . C31 C 0.0001(11) 0.45283(16) 0.7169(5) 0.066(3) Uani 1 1 d . . . H31A H -0.0622 0.4684 0.7187 0.099 Uiso 1 1 calc R . . H31B H -0.0164 0.4443 0.6730 0.099 Uiso 1 1 calc R . . H31C H 0.1091 0.4573 0.7217 0.099 Uiso 1 1 calc R . . C32 C 0.6576(7) 0.39328(13) 0.6592(4) 0.0377(16) Uani 1 1 d . . . H32A H 0.6593 0.4110 0.6414 0.045 Uiso 1 1 calc R . . H32B H 0.7598 0.3855 0.6509 0.045 Uiso 1 1 calc R . . C33 C 0.6248(7) 0.39359(13) 0.7337(3) 0.0356(16) Uani 1 1 d . . . H33A H 0.6476 0.3767 0.7538 0.043 Uiso 1 1 calc R . . H33B H 0.6904 0.4064 0.7566 0.043 Uiso 1 1 calc R . . C34 C 0.5721(10) 0.3766(2) 0.5525(4) 0.069(3) Uani 1 1 d . . . H34A H 0.5878 0.3936 0.5328 0.104 Uiso 1 1 calc R . . H34B H 0.4841 0.3684 0.5302 0.104 Uiso 1 1 calc R . . H34C H 0.6645 0.3662 0.5455 0.104 Uiso 1 1 calc R . . C35 C 0.4329(8) 0.40808(14) 0.8125(3) 0.0390(16) Uani 1 1 d . . . H35A H 0.4654 0.3950 0.8451 0.059 Uiso 1 1 calc R . . H35B H 0.3219 0.4110 0.8170 0.059 Uiso 1 1 calc R . . H35C H 0.4880 0.4240 0.8220 0.059 Uiso 1 1 calc R . . C36 C 0.4185(16) 0.2034(3) 0.9221(7) 0.116(4) Uiso 1 1 d D . . C37 C 0.3271(14) 0.1973(2) 0.9801(7) 0.104(4) Uiso 1 1 d D . . H37 H 0.3609 0.1865 1.0160 0.125 Uiso 1 1 calc R . . C38 C 0.1879(15) 0.2084(3) 0.9789(7) 0.112(4) Uiso 1 1 d D . . H38 H 0.1241 0.2045 1.0169 0.134 Uiso 1 1 calc R . . C39 C 0.1221(18) 0.2247(3) 0.9316(7) 0.117(5) Uiso 1 1 d . . . H39 H 0.0217 0.2317 0.9357 0.140 Uiso 1 1 calc R . . C40 C 0.2211(16) 0.2295(3) 0.8773(8) 0.124(5) Uiso 1 1 d D . . H40 H 0.1887 0.2409 0.8424 0.149 Uiso 1 1 calc R . . C41 C 0.3628(16) 0.2185(2) 0.8722(7) 0.114(4) Uiso 1 1 d D . . H41 H 0.4236 0.2216 0.8327 0.137 Uiso 1 1 calc R . . C42 C 0.5763(19) 0.1936(3) 0.9199(10) 0.172(7) Uiso 1 1 d D . . H42A H 0.5986 0.1871 0.8740 0.257 Uiso 1 1 calc R . . H42B H 0.5877 0.1798 0.9533 0.257 Uiso 1 1 calc R . . H42C H 0.6481 0.2074 0.9310 0.257 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0223(3) 0.0232(3) 0.0232(3) 0.0004(3) -0.0038(2) 0.0002(2) Si1 0.0380(11) 0.0296(10) 0.0493(12) 0.0082(9) -0.0060(9) 0.0065(8) Si2 0.0297(9) 0.0248(9) 0.0307(9) 0.0016(7) -0.0036(7) -0.0040(7) O1 0.027(2) 0.048(3) 0.040(3) -0.003(2) 0.006(2) 0.009(2) O2 0.029(2) 0.047(3) 0.027(2) -0.008(2) 0.0006(19) 0.001(2) O3 0.023(2) 0.040(2) 0.020(2) -0.0063(18) -0.0010(17) 0.0017(19) N1 0.040(3) 0.020(3) 0.033(3) 0.003(2) -0.002(3) -0.002(2) N2 0.069(5) 0.024(3) 0.060(4) 0.004(3) -0.040(4) -0.013(3) N3 0.032(3) 0.023(3) 0.025(3) 0.003(2) -0.005(2) -0.005(2) N4 0.079(4) 0.031(2) 0.032(2) 0.000(2) -0.028(2) -0.021(2) C1 0.041(4) 0.023(3) 0.039(4) -0.002(3) 0.000(3) -0.003(3) C2 0.079(4) 0.031(2) 0.032(2) 0.000(2) -0.028(2) -0.021(2) C3 0.089(4) 0.067(4) 0.059(3) 0.012(3) -0.042(3) -0.036(3) C4 0.089(4) 0.067(4) 0.059(3) 0.012(3) -0.042(3) -0.036(3) C5 0.089(4) 0.067(4) 0.059(3) 0.012(3) -0.042(3) -0.036(3) C6 0.035(4) 0.027(4) 0.050(4) 0.002(3) -0.010(3) 0.004(3) C7 0.049(5) 0.054(5) 0.081(6) -0.024(5) 0.002(4) 0.007(4) C8 0.077(7) 0.044(5) 0.111(9) -0.029(6) -0.025(6) 0.026(5) C9 0.088(8) 0.031(5) 0.151(11) -0.013(6) -0.051(8) -0.002(5) C10 0.055(5) 0.044(5) 0.128(9) 0.020(6) -0.019(6) -0.020(4) C11 0.041(4) 0.044(4) 0.076(6) 0.004(4) 0.006(4) -0.005(3) C12 0.031(4) 0.026(3) 0.024(3) -0.001(3) -0.005(3) -0.007(3) C13 0.032(4) 0.030(3) 0.027(3) 0.000(3) -0.003(3) 0.002(3) C14 0.059(5) 0.039(4) 0.021(3) 0.007(3) 0.000(3) -0.004(4) C15 0.071(6) 0.029(4) 0.040(4) 0.000(3) -0.024(4) 0.012(4) C16 0.042(4) 0.053(5) 0.047(5) -0.007(4) -0.011(4) 0.013(4) C17 0.034(4) 0.053(5) 0.032(4) -0.005(3) 0.002(3) 0.001(3) C18 0.087(7) 0.035(5) 0.081(7) 0.017(4) -0.012(6) -0.004(4) C19 0.072(6) 0.057(5) 0.053(5) 0.012(4) -0.018(4) 0.003(4) C20 0.046(5) 0.064(6) 0.089(7) 0.006(5) 0.006(5) 0.029(4) C21 0.057(5) 0.030(4) 0.055(5) -0.002(3) -0.014(4) 0.005(3) C22 0.047(4) 0.042(4) 0.050(5) 0.005(3) 0.004(4) -0.016(4) C23 0.056(5) 0.043(4) 0.037(4) -0.004(3) -0.009(3) -0.020(4) C24 0.021(3) 0.051(4) 0.026(3) -0.011(3) -0.006(3) 0.003(3) C25 0.027(3) 0.063(5) 0.034(4) 0.002(3) -0.009(3) 0.004(3) C26 0.034(4) 0.117(8) 0.028(4) 0.009(5) -0.006(3) -0.009(5) C27 0.034(4) 0.120(9) 0.036(5) -0.038(5) -0.003(4) -0.003(5) C28 0.034(4) 0.067(5) 0.058(6) -0.038(5) -0.007(4) 0.003(4) C29 0.026(4) 0.049(4) 0.050(4) -0.020(4) -0.008(3) 0.001(3) C30 0.066(6) 0.092(7) 0.089(8) 0.048(6) 0.007(6) 0.009(6) C31 0.061(6) 0.046(5) 0.091(7) 0.001(5) -0.003(5) 0.000(4) C32 0.025(3) 0.048(4) 0.039(4) 0.000(3) 0.010(3) -0.002(3) C33 0.025(3) 0.046(4) 0.036(4) -0.003(3) -0.005(3) 0.003(3) C34 0.056(5) 0.114(8) 0.038(5) -0.022(5) 0.008(4) 0.015(5) C35 0.040(4) 0.053(4) 0.023(3) -0.008(3) 0.000(3) 0.003(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 Y1 O1 2.105(4) . ? Y1 N4 2.317(6) . ? Y1 N2 2.319(5) . ? Y1 O3 2.392(4) . ? Y1 O2 2.446(4) . ? Y1 N1 2.516(5) . ? Y1 N3 2.524(5) . ? Y1 C2 2.820(7) . ? Y1 C1 2.832(6) . ? Si1 N1 1.733(5) . ? Si1 C19 1.860(8) . ? Si1 C20 1.879(8) . ? Si1 C18 1.886(8) . ? Si2 N3 1.722(5) . ? Si2 C21 1.863(7) . ? Si2 C23 1.868(7) . ? Si2 C22 1.877(7) . ? O1 C24 1.326(7) . ? O2 C32 1.423(8) . ? O2 C34 1.441(8) . ? O3 C33 1.420(7) . ? O3 C35 1.448(7) . ? N1 C1 1.330(8) . ? N2 C1 1.318(8) . ? N2 C3 1.466(9) . ? N3 C2 1.335(8) . ? N4 C2 1.296(8) . ? N4 C5 1.449(9) . ? C1 C6 1.501(9) . ? C2 C12 1.502(9) . ? C3 C4 1.475(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.438(10) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.372(10) . ? C6 C11 1.380(10) . ? C7 C8 1.397(12) . ? C7 H7 0.9500 . ? C8 C9 1.366(15) . ? C8 H8 0.9500 . ? C9 C10 1.363(15) . ? C9 H9 0.9500 . ? C10 C11 1.386(11) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.384(8) . ? C12 C17 1.393(9) . ? C13 C14 1.383(9) . ? C13 H13 0.9500 . ? C14 C15 1.373(11) . ? C14 H14 0.9500 . ? C15 C16 1.380(11) . ? C15 H15 0.9500 . ? C16 C17 1.382(10) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? 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 C25 1.374(10) . ? C24 C29 1.413(10) . ? C25 C26 1.395(11) . ? C25 C30 1.530(12) . ? C26 C27 1.361(13) . ? C26 H26 0.9500 . ? C27 C28 1.375(12) . ? C27 H27 0.9500 . ? C28 C29 1.394(10) . ? C28 H28 0.9500 . ? C29 C31 1.483(11) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.486(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C41 1.350(13) . ? C36 C37 1.422(13) . ? C36 C42 1.464(14) . ? C37 C38 1.344(13) . ? C37 H37 0.9500 . ? C38 C39 1.382(17) . ? C38 H38 0.9500 . ? C39 C40 1.390(18) . ? C39 H39 0.9500 . ? C40 C41 1.364(13) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 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 O1 Y1 N4 109.2(2) . . ? O1 Y1 N2 96.8(2) . . ? N4 Y1 N2 73.7(2) . . ? O1 Y1 O3 88.28(16) . . ? N4 Y1 O3 137.66(18) . . ? N2 Y1 O3 144.11(18) . . ? O1 Y1 O2 154.65(16) . . ? N4 Y1 O2 89.9(2) . . ? N2 Y1 O2 104.7(2) . . ? O3 Y1 O2 66.42(14) . . ? O1 Y1 N1 102.68(18) . . ? N4 Y1 N1 122.17(18) . . ? N2 Y1 N1 55.32(19) . . ? O3 Y1 N1 88.87(16) . . ? O2 Y1 N1 79.48(16) . . ? O1 Y1 N3 97.23(18) . . ? N4 Y1 N3 54.77(17) . . ? N2 Y1 N3 128.42(18) . . ? O3 Y1 N3 85.67(15) . . ? O2 Y1 N3 79.92(16) . . ? N1 Y1 N3 159.18(17) . . ? O1 Y1 C2 101.3(2) . . ? N4 Y1 C2 27.02(18) . . ? N2 Y1 C2 100.2(2) . . ? O3 Y1 C2 113.62(17) . . ? O2 Y1 C2 88.1(2) . . ? N1 Y1 C2 147.46(19) . . ? N3 Y1 C2 28.24(17) . . ? O1 Y1 C1 102.67(19) . . ? N4 Y1 C1 97.10(19) . . ? N2 Y1 C1 27.40(19) . . ? O3 Y1 C1 116.88(17) . . ? O2 Y1 C1 90.93(17) . . ? N1 Y1 C1 28.01(18) . . ? N3 Y1 C1 149.99(18) . . ? C2 Y1 C1 124.07(19) . . ? N1 Si1 C19 108.4(3) . . ? N1 Si1 C20 110.2(3) . . ? C19 Si1 C20 108.2(4) . . ? N1 Si1 C18 117.2(4) . . ? C19 Si1 C18 105.9(4) . . ? C20 Si1 C18 106.7(4) . . ? N3 Si2 C21 116.1(3) . . ? N3 Si2 C23 108.8(3) . . ? C21 Si2 C23 106.3(4) . . ? N3 Si2 C22 111.8(3) . . ? C21 Si2 C22 106.6(4) . . ? C23 Si2 C22 106.6(4) . . ? C24 O1 Y1 172.3(4) . . ? C32 O2 C34 112.5(6) . . ? C32 O2 Y1 114.9(3) . . ? C34 O2 Y1 117.7(4) . . ? C33 O3 C35 113.3(5) . . ? C33 O3 Y1 120.8(3) . . ? C35 O3 Y1 124.7(4) . . ? C1 N1 Si1 126.9(4) . . ? C1 N1 Y1 89.3(4) . . ? Si1 N1 Y1 142.2(3) . . ? C1 N2 C3 121.8(6) . . ? C1 N2 Y1 98.5(4) . . ? C3 N2 Y1 138.4(5) . . ? C2 N3 Si2 126.5(4) . . ? C2 N3 Y1 88.3(4) . . ? Si2 N3 Y1 145.0(3) . . ? C2 N4 C5 123.1(6) . . ? C2 N4 Y1 98.7(4) . . ? C5 N4 Y1 136.7(5) . . ? N2 C1 N1 116.5(6) . . ? N2 C1 C6 120.1(6) . . ? N1 C1 C6 123.4(6) . . ? N2 C1 Y1 54.1(3) . . ? N1 C1 Y1 62.7(3) . . ? C6 C1 Y1 172.6(5) . . ? N4 C2 N3 116.3(6) . . ? N4 C2 C12 121.3(6) . . ? N3 C2 C12 122.4(6) . . ? N4 C2 Y1 54.3(4) . . ? N3 C2 Y1 63.5(3) . . ? C12 C2 Y1 165.8(6) . . ? N2 C3 C4 112.7(7) . . ? N2 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? N2 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 122.3(9) . . ? C5 C4 H4A 106.7 . . ? C3 C4 H4A 106.7 . . ? C5 C4 H4B 106.7 . . ? C3 C4 H4B 106.7 . . ? H4A C4 H4B 106.6 . . ? C4 C5 N4 112.9(7) . . ? C4 C5 H5A 109.0 . . ? N4 C5 H5A 109.0 . . ? C4 C5 H5B 109.0 . . ? N4 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C7 C6 C11 118.9(7) . . ? C7 C6 C1 121.6(7) . . ? C11 C6 C1 119.5(7) . . ? C6 C7 C8 121.1(9) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C7 119.2(10) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C10 C9 C8 119.9(9) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 121.2(9) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C6 C11 C10 119.6(8) . . ? C6 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C17 118.6(6) . . ? C13 C12 C2 121.5(6) . . ? C17 C12 C2 119.9(6) . . ? C14 C13 C12 120.1(6) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.8(7) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.8(7) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 119.7(7) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C12 120.8(7) . . ? C16 C17 H17 119.6 . . ? C12 C17 H17 119.6 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O1 C24 C25 120.6(6) . . ? O1 C24 C29 119.5(6) . . ? C25 C24 C29 120.0(6) . . ? C24 C25 C26 120.2(7) . . ? C24 C25 C30 120.6(7) . . ? C26 C25 C30 119.2(8) . . ? C27 C26 C25 120.5(8) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 119.8(8) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C29 121.5(8) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C28 C29 C24 118.0(8) . . ? C28 C29 C31 122.6(8) . . ? C24 C29 C31 119.4(7) . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O2 C32 C33 109.6(5) . . ? O2 C32 H32A 109.8 . . ? C33 C32 H32A 109.8 . . ? O2 C32 H32B 109.8 . . ? C33 C32 H32B 109.8 . . ? H32A C32 H32B 108.2 . . ? O3 C33 C32 108.8(5) . . ? O3 C33 H33A 109.9 . . ? C32 C33 H33A 109.9 . . ? O3 C33 H33B 109.9 . . ? C32 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? O2 C34 H34A 109.5 . . ? O2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O3 C35 H35A 109.5 . . ? O3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 C36 C37 120.6(14) . . ? C41 C36 C42 121.4(14) . . ? C37 C36 C42 117.9(14) . . ? C38 C37 C36 113.1(13) . . ? C38 C37 H37 123.5 . . ? C36 C37 H37 123.5 . . ? C37 C38 C39 130.7(15) . . ? C37 C38 H38 114.7 . . ? C39 C38 H38 114.7 . . ? C38 C39 C40 111.7(14) . . ? C38 C39 H39 124.2 . . ? C40 C39 H39 124.2 . . ? C41 C40 C39 122.5(15) . . ? C41 C40 H40 118.7 . . ? C39 C40 H40 118.7 . . ? C36 C41 C40 121.3(15) . . ? C36 C41 H41 119.3 . . ? C40 C41 H41 119.3 . . ? C36 C42 H42A 109.5 . . ? C36 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C36 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 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 N4 Y1 O1 C24 177(100) . . . . ? N2 Y1 O1 C24 102(3) . . . . ? O3 Y1 O1 C24 -42(3) . . . . ? O2 Y1 O1 C24 -46(4) . . . . ? N1 Y1 O1 C24 46(3) . . . . ? N3 Y1 O1 C24 -128(3) . . . . ? C2 Y1 O1 C24 -156(3) . . . . ? C1 Y1 O1 C24 75(3) . . . . ? O1 Y1 O2 C32 -17.9(7) . . . . ? N4 Y1 O2 C32 121.9(4) . . . . ? N2 Y1 O2 C32 -165.0(4) . . . . ? O3 Y1 O2 C32 -21.9(4) . . . . ? N1 Y1 O2 C32 -115.3(4) . . . . ? N3 Y1 O2 C32 67.7(4) . . . . ? C2 Y1 O2 C32 94.9(4) . . . . ? C1 Y1 O2 C32 -141.0(4) . . . . ? O1 Y1 O2 C34 -153.9(6) . . . . ? N4 Y1 O2 C34 -14.2(6) . . . . ? N2 Y1 O2 C34 59.0(6) . . . . ? O3 Y1 O2 C34 -158.0(6) . . . . ? N1 Y1 O2 C34 108.6(6) . . . . ? N3 Y1 O2 C34 -68.3(6) . . . . ? C2 Y1 O2 C34 -41.1(6) . . . . ? C1 Y1 O2 C34 82.9(6) . . . . ? O1 Y1 O3 C33 176.3(5) . . . . ? N4 Y1 O3 C33 -66.7(5) . . . . ? N2 Y1 O3 C33 77.1(6) . . . . ? O2 Y1 O3 C33 -5.4(4) . . . . ? N1 Y1 O3 C33 73.6(5) . . . . ? N3 Y1 O3 C33 -86.3(5) . . . . ? C2 Y1 O3 C33 -82.1(5) . . . . ? C1 Y1 O3 C33 73.0(5) . . . . ? O1 Y1 O3 C35 9.8(5) . . . . ? N4 Y1 O3 C35 126.8(5) . . . . ? N2 Y1 O3 C35 -89.4(6) . . . . ? O2 Y1 O3 C35 -171.9(5) . . . . ? N1 Y1 O3 C35 -92.9(5) . . . . ? N3 Y1 O3 C35 107.2(5) . . . . ? C2 Y1 O3 C35 111.4(5) . . . . ? C1 Y1 O3 C35 -93.5(5) . . . . ? C19 Si1 N1 C1 -149.6(6) . . . . ? C20 Si1 N1 C1 92.2(7) . . . . ? C18 Si1 N1 C1 -30.0(7) . . . . ? C19 Si1 N1 Y1 50.2(6) . . . . ? C20 Si1 N1 Y1 -68.0(6) . . . . ? C18 Si1 N1 Y1 169.9(5) . . . . ? O1 Y1 N1 C1 93.2(4) . . . . ? N4 Y1 N1 C1 -29.4(5) . . . . ? N2 Y1 N1 C1 3.7(4) . . . . ? O3 Y1 N1 C1 -178.8(4) . . . . ? O2 Y1 N1 C1 -112.6(4) . . . . ? N3 Y1 N1 C1 -104.1(5) . . . . ? C2 Y1 N1 C1 -43.3(6) . . . . ? O1 Y1 N1 Si1 -102.5(5) . . . . ? N4 Y1 N1 Si1 134.9(5) . . . . ? N2 Y1 N1 Si1 168.0(6) . . . . ? O3 Y1 N1 Si1 -14.5(5) . . . . ? O2 Y1 N1 Si1 51.7(5) . . . . ? N3 Y1 N1 Si1 60.1(7) . . . . ? C2 Y1 N1 Si1 121.0(5) . . . . ? C1 Y1 N1 Si1 164.3(7) . . . . ? O1 Y1 N2 C1 -104.5(5) . . . . ? N4 Y1 N2 C1 147.4(5) . . . . ? O3 Y1 N2 C1 -8.1(7) . . . . ? O2 Y1 N2 C1 61.9(5) . . . . ? N1 Y1 N2 C1 -3.8(4) . . . . ? N3 Y1 N2 C1 150.6(4) . . . . ? C2 Y1 N2 C1 152.7(5) . . . . ? O1 Y1 N2 C3 89.5(9) . . . . ? N4 Y1 N2 C3 -18.5(9) . . . . ? O3 Y1 N2 C3 -174.0(8) . . . . ? O2 Y1 N2 C3 -104.0(9) . . . . ? N1 Y1 N2 C3 -169.7(10) . . . . ? N3 Y1 N2 C3 -15.3(11) . . . . ? C2 Y1 N2 C3 -13.3(10) . . . . ? C1 Y1 N2 C3 -165.9(13) . . . . ? C21 Si2 N3 C2 44.6(8) . . . . ? C23 Si2 N3 C2 164.4(7) . . . . ? C22 Si2 N3 C2 -78.1(7) . . . . ? C21 Si2 N3 Y1 -128.4(5) . . . . ? C23 Si2 N3 Y1 -8.5(6) . . . . ? C22 Si2 N3 Y1 109.0(5) . . . . ? O1 Y1 N3 C2 -100.4(5) . . . . ? N4 Y1 N3 C2 8.0(5) . . . . ? N2 Y1 N3 C2 4.2(6) . . . . ? O3 Y1 N3 C2 171.9(5) . . . . ? O2 Y1 N3 C2 105.1(5) . . . . ? N1 Y1 N3 C2 96.7(6) . . . . ? C1 Y1 N3 C2 31.1(6) . . . . ? O1 Y1 N3 Si2 74.0(5) . . . . ? N4 Y1 N3 Si2 -177.7(6) . . . . ? N2 Y1 N3 Si2 178.6(5) . . . . ? O3 Y1 N3 Si2 -13.8(5) . . . . ? O2 Y1 N3 Si2 -80.6(5) . . . . ? N1 Y1 N3 Si2 -89.0(7) . . . . ? C2 Y1 N3 Si2 174.3(8) . . . . ? C1 Y1 N3 Si2 -154.6(4) . . . . ? O1 Y1 N4 C2 76.9(6) . . . . ? N2 Y1 N4 C2 168.6(6) . . . . ? O3 Y1 N4 C2 -32.6(7) . . . . ? O2 Y1 N4 C2 -86.0(6) . . . . ? N1 Y1 N4 C2 -163.5(5) . . . . ? N3 Y1 N4 C2 -8.3(5) . . . . ? C1 Y1 N4 C2 -177.0(6) . . . . ? O1 Y1 N4 C5 -88.7(9) . . . . ? N2 Y1 N4 C5 2.9(9) . . . . ? O3 Y1 N4 C5 161.8(8) . . . . ? O2 Y1 N4 C5 108.3(9) . . . . ? N1 Y1 N4 C5 30.8(10) . . . . ? N3 Y1 N4 C5 -174.0(10) . . . . ? C2 Y1 N4 C5 -165.7(13) . . . . ? C1 Y1 N4 C5 17.4(9) . . . . ? C3 N2 C1 N1 175.6(7) . . . . ? Y1 N2 C1 N1 6.6(7) . . . . ? C3 N2 C1 C6 -5.5(12) . . . . ? Y1 N2 C1 C6 -174.6(5) . . . . ? C3 N2 C1 Y1 169.1(10) . . . . ? Si1 N1 C1 N2 -174.0(5) . . . . ? Y1 N1 C1 N2 -6.0(7) . . . . ? Si1 N1 C1 C6 7.2(10) . . . . ? Y1 N1 C1 C6 175.2(6) . . . . ? Si1 N1 C1 Y1 -168.0(6) . . . . ? O1 Y1 C1 N2 80.1(5) . . . . ? N4 Y1 C1 N2 -31.4(5) . . . . ? O3 Y1 C1 N2 174.7(5) . . . . ? O2 Y1 C1 N2 -121.4(5) . . . . ? N1 Y1 C1 N2 173.4(7) . . . . ? N3 Y1 C1 N2 -50.2(7) . . . . ? C2 Y1 C1 N2 -33.0(6) . . . . ? O1 Y1 C1 N1 -93.2(4) . . . . ? N4 Y1 C1 N1 155.2(4) . . . . ? N2 Y1 C1 N1 -173.4(7) . . . . ? O3 Y1 C1 N1 1.3(4) . . . . ? O2 Y1 C1 N1 65.2(4) . . . . ? N3 Y1 C1 N1 136.4(4) . . . . ? C2 Y1 C1 N1 153.6(4) . . . . ? O1 Y1 C1 C6 120(4) . . . . ? N4 Y1 C1 C6 8(4) . . . . ? N2 Y1 C1 C6 40(4) . . . . ? O3 Y1 C1 C6 -146(4) . . . . ? O2 Y1 C1 C6 -82(4) . . . . ? N1 Y1 C1 C6 -147(4) . . . . ? N3 Y1 C1 C6 -10(4) . . . . ? C2 Y1 C1 C6 7(4) . . . . ? C5 N4 C2 N3 -177.2(8) . . . . ? Y1 N4 C2 N3 14.5(9) . . . . ? C5 N4 C2 C12 4.5(14) . . . . ? Y1 N4 C2 C12 -163.9(7) . . . . ? C5 N4 C2 Y1 168.3(10) . . . . ? Si2 N3 C2 N4 170.9(6) . . . . ? Y1 N3 C2 N4 -13.1(8) . . . . ? Si2 N3 C2 C12 -10.8(11) . . . . ? Y1 N3 C2 C12 165.2(7) . . . . ? Si2 N3 C2 Y1 -176.0(6) . . . . ? O1 Y1 C2 N4 -110.2(6) . . . . ? N2 Y1 C2 N4 -11.1(6) . . . . ? O3 Y1 C2 N4 156.7(5) . . . . ? O2 Y1 C2 N4 93.5(6) . . . . ? N1 Y1 C2 N4 26.5(8) . . . . ? N3 Y1 C2 N4 165.5(9) . . . . ? C1 Y1 C2 N4 3.6(7) . . . . ? O1 Y1 C2 N3 84.3(5) . . . . ? N4 Y1 C2 N3 -165.5(9) . . . . ? N2 Y1 C2 N3 -176.6(4) . . . . ? O3 Y1 C2 N3 -8.8(5) . . . . ? O2 Y1 C2 N3 -72.0(4) . . . . ? N1 Y1 C2 N3 -139.0(4) . . . . ? C1 Y1 C2 N3 -161.9(4) . . . . ? O1 Y1 C2 C12 -33.8(18) . . . . ? N4 Y1 C2 C12 76.4(18) . . . . ? N2 Y1 C2 C12 65.3(18) . . . . ? O3 Y1 C2 C12 -126.9(18) . . . . ? O2 Y1 C2 C12 169.9(18) . . . . ? N1 Y1 C2 C12 102.9(19) . . . . ? N3 Y1 C2 C12 -118(2) . . . . ? C1 Y1 C2 C12 80.1(19) . . . . ? C1 N2 C3 C4 -163.3(9) . . . . ? Y1 N2 C3 C4 0.3(15) . . . . ? N2 C3 C4 C5 46.3(14) . . . . ? C3 C4 C5 N4 -59.4(13) . . . . ? C2 N4 C5 C4 -134.5(10) . . . . ? Y1 N4 C5 C4 28.5(14) . . . . ? N2 C1 C6 C7 95.1(9) . . . . ? N1 C1 C6 C7 -86.2(10) . . . . ? Y1 C1 C6 C7 58(4) . . . . ? N2 C1 C6 C11 -84.2(9) . . . . ? N1 C1 C6 C11 94.5(9) . . . . ? Y1 C1 C6 C11 -121(4) . . . . ? C11 C6 C7 C8 -1.5(13) . . . . ? C1 C6 C7 C8 179.2(8) . . . . ? C6 C7 C8 C9 -0.5(15) . . . . ? C7 C8 C9 C10 1.6(16) . . . . ? C8 C9 C10 C11 -0.7(16) . . . . ? C7 C6 C11 C10 2.4(12) . . . . ? C1 C6 C11 C10 -178.3(8) . . . . ? C9 C10 C11 C6 -1.3(14) . . . . ? N4 C2 C12 C13 -95.7(10) . . . . ? N3 C2 C12 C13 86.1(10) . . . . ? Y1 C2 C12 C13 -163.2(15) . . . . ? N4 C2 C12 C17 82.4(10) . . . . ? N3 C2 C12 C17 -95.9(9) . . . . ? Y1 C2 C12 C17 15(2) . . . . ? C17 C12 C13 C14 3.4(9) . . . . ? C2 C12 C13 C14 -178.5(6) . . . . ? C12 C13 C14 C15 -1.5(10) . . . . ? C13 C14 C15 C16 -0.7(11) . . . . ? C14 C15 C16 C17 0.9(11) . . . . ? C15 C16 C17 C12 1.1(11) . . . . ? C13 C12 C17 C16 -3.3(10) . . . . ? C2 C12 C17 C16 178.6(6) . . . . ? Y1 O1 C24 C25 -42(4) . . . . ? Y1 O1 C24 C29 139(3) . . . . ? O1 C24 C25 C26 180.0(6) . . . . ? C29 C24 C25 C26 -0.9(10) . . . . ? O1 C24 C25 C30 -2.3(10) . . . . ? C29 C24 C25 C30 176.8(7) . . . . ? C24 C25 C26 C27 -0.2(11) . . . . ? C30 C25 C26 C27 -178.0(8) . . . . ? C25 C26 C27 C28 1.3(12) . . . . ? C26 C27 C28 C29 -1.3(11) . . . . ? C27 C28 C29 C24 0.2(10) . . . . ? C27 C28 C29 C31 179.0(7) . . . . ? O1 C24 C29 C28 -180.0(6) . . . . ? C25 C24 C29 C28 0.9(9) . . . . ? O1 C24 C29 C31 1.1(10) . . . . ? C25 C24 C29 C31 -178.0(7) . . . . ? C34 O2 C32 C33 -176.5(6) . . . . ? Y1 O2 C32 C33 45.2(6) . . . . ? C35 O3 C33 C32 -162.3(5) . . . . ? Y1 O3 C33 C32 29.8(7) . . . . ? O2 C32 C33 O3 -47.4(7) . . . . ? C41 C36 C37 C38 -1(2) . . . . ? C42 C36 C37 C38 176.1(14) . . . . ? C36 C37 C38 C39 -1(2) . . . . ? C37 C38 C39 C40 0(2) . . . . ? C38 C39 C40 C41 2(2) . . . . ? C37 C36 C41 C40 3(2) . . . . ? C42 C36 C41 C40 -173.8(15) . . . . ? C39 C40 C41 C36 -4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.012 _refine_diff_density_min -1.904 _refine_diff_density_rms 0.098 data_complex4 _database_code_depnum_ccdc_archive 'CCDC 915746' #TrackingRef '915746.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H67 N4 Nd O3 Si2' _chemical_formula_sum 'C42 H67 N4 Nd O3 Si2' _chemical_formula_weight 876.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 9.0793(2) _cell_length_b 14.3645(3) _cell_length_c 33.6538(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.124(2) _cell_angle_gamma 90.00 _cell_volume 4371.59(17) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 10362 _cell_measurement_theta_min 3.3340 _cell_measurement_theta_max 29.2430 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1836 _exptl_absorpt_coefficient_mu 1.283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.92124 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3818 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29627 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_unetI/netI 0.0503 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8114 _reflns_number_gt 6683 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+1.8018P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8114 _refine_ls_number_parameters 484 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0653 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.124417(18) 0.760712(10) 0.861862(5) 0.01419(6) Uani 1 1 d . . . Si1 Si 0.28974(10) 0.56867(6) 0.94196(3) 0.0195(2) Uani 1 1 d . . . Si2 Si 0.31742(11) 0.90861(6) 0.77167(3) 0.0238(2) Uani 1 1 d . . . O1 O -0.0259(2) 0.85977(13) 0.88826(6) 0.0177(5) Uani 1 1 d . . . O2 O 0.3959(2) 0.70927(13) 0.86471(6) 0.0201(5) Uani 1 1 d . . . O3 O 0.3281(2) 0.87158(13) 0.89465(6) 0.0205(5) Uani 1 1 d . . . N1 N 0.1620(3) 0.61696(16) 0.90653(7) 0.0171(6) Uani 1 1 d . . . N2 N -0.0432(3) 0.62804(17) 0.86370(8) 0.0211(6) Uani 1 1 d . . . N3 N 0.2056(3) 0.82941(16) 0.79327(7) 0.0194(6) Uani 1 1 d . . . N4 N 0.0273(3) 0.72016(19) 0.79474(8) 0.0274(7) Uani 1 1 d . . . C1 C 0.0416(4) 0.57651(19) 0.88821(9) 0.0173(7) Uani 1 1 d . . . C2 C 0.1002(4) 0.7780(2) 0.77346(9) 0.0202(7) Uani 1 1 d . . . C3 C -0.1693(4) 0.5882(2) 0.83950(10) 0.0279(8) Uani 1 1 d . . . H3A H -0.2547 0.5836 0.8557 0.033 Uiso 1 1 calc R . . H3B H -0.1442 0.5246 0.8311 0.033 Uiso 1 1 calc R . . C4 C -0.2111(4) 0.6466(2) 0.80328(10) 0.0297(8) Uani 1 1 d . . . H4A H -0.2435 0.7085 0.8121 0.036 Uiso 1 1 calc R . . H4B H -0.2965 0.6172 0.7878 0.036 Uiso 1 1 calc R . . C5 C -0.0895(4) 0.6600(3) 0.77635(10) 0.0384(10) Uani 1 1 d . . . H5A H -0.0469 0.5988 0.7703 0.046 Uiso 1 1 calc R . . H5B H -0.1309 0.6881 0.7509 0.046 Uiso 1 1 calc R . . C6 C 0.0017(4) 0.4766(2) 0.89518(9) 0.0182(7) Uani 1 1 d . . . C7 C 0.0762(4) 0.4042(2) 0.87876(10) 0.0269(8) Uani 1 1 d . . . H7 H 0.1546 0.4169 0.8627 0.032 Uiso 1 1 calc R . . C8 C 0.0362(4) 0.3129(2) 0.88585(11) 0.0346(9) Uani 1 1 d . . . H8 H 0.0873 0.2633 0.8744 0.042 Uiso 1 1 calc R . . C9 C -0.0762(4) 0.2934(2) 0.90912(11) 0.0345(9) Uani 1 1 d . . . H9 H -0.1020 0.2307 0.9141 0.041 Uiso 1 1 calc R . . C10 C -0.1514(4) 0.3651(2) 0.92522(10) 0.0296(8) Uani 1 1 d . . . H10 H -0.2295 0.3519 0.9413 0.035 Uiso 1 1 calc R . . C11 C -0.1137(4) 0.4570(2) 0.91806(9) 0.0252(8) Uani 1 1 d . . . H11 H -0.1672 0.5063 0.9289 0.030 Uiso 1 1 calc R . . C12 C 0.0633(4) 0.7844(2) 0.72899(9) 0.0206(7) Uani 1 1 d . . . C13 C -0.0586(4) 0.8341(2) 0.71299(10) 0.0336(9) Uani 1 1 d . . . H13 H -0.1193 0.8655 0.7303 0.040 Uiso 1 1 calc R . . C14 C -0.0933(5) 0.8386(2) 0.67220(11) 0.0387(10) Uani 1 1 d . . . H14 H -0.1764 0.8738 0.6617 0.046 Uiso 1 1 calc R . . C15 C -0.0092(4) 0.7927(2) 0.64683(10) 0.0349(10) Uani 1 1 d . . . H15 H -0.0333 0.7963 0.6188 0.042 Uiso 1 1 calc R . . C16 C 0.1107(4) 0.7414(2) 0.66202(10) 0.0346(9) Uani 1 1 d . . . H16 H 0.1684 0.7085 0.6445 0.041 Uiso 1 1 calc R . . C17 C 0.1476(4) 0.7376(2) 0.70313(9) 0.0251(7) Uani 1 1 d . . . H17 H 0.2313 0.7026 0.7134 0.030 Uiso 1 1 calc R . . C18 C 0.2083(4) 0.4910(2) 0.97849(10) 0.0361(9) Uani 1 1 d . . . H18A H 0.1248 0.5226 0.9893 0.054 Uiso 1 1 calc R . . H18B H 0.2835 0.4762 1.0003 0.054 Uiso 1 1 calc R . . H18C H 0.1737 0.4334 0.9651 0.054 Uiso 1 1 calc R . . C19 C 0.3830(4) 0.6659(2) 0.97097(10) 0.0303(8) Uani 1 1 d . . . H19A H 0.4254 0.7093 0.9526 0.045 Uiso 1 1 calc R . . H19B H 0.4619 0.6408 0.9897 0.045 Uiso 1 1 calc R . . H19C H 0.3107 0.6986 0.9858 0.045 Uiso 1 1 calc R . . C20 C 0.4398(4) 0.5014(3) 0.92039(11) 0.0425(10) Uani 1 1 d . . . H20A H 0.3959 0.4527 0.9027 0.064 Uiso 1 1 calc R . . H20B H 0.5038 0.4728 0.9420 0.064 Uiso 1 1 calc R . . H20C H 0.4984 0.5435 0.9052 0.064 Uiso 1 1 calc R . . C21 C 0.2206(5) 0.9868(2) 0.73346(11) 0.0418(10) Uani 1 1 d . . . H21A H 0.1879 0.9505 0.7096 0.063 Uiso 1 1 calc R . . H21B H 0.2885 1.0358 0.7263 0.063 Uiso 1 1 calc R . . H21C H 0.1346 1.0150 0.7444 0.063 Uiso 1 1 calc R . . C22 C 0.4715(4) 0.8513(3) 0.74712(10) 0.0350(9) Uani 1 1 d . . . H22A H 0.5268 0.8101 0.7663 0.053 Uiso 1 1 calc R . . H22B H 0.5380 0.8991 0.7381 0.053 Uiso 1 1 calc R . . H22C H 0.4302 0.8149 0.7242 0.053 Uiso 1 1 calc R . . C23 C 0.4038(4) 0.9887(2) 0.81080(10) 0.0254(8) Uani 1 1 d . . . H23A H 0.3271 1.0141 0.8264 0.038 Uiso 1 1 calc R . . H23B H 0.4534 1.0399 0.7980 0.038 Uiso 1 1 calc R . . H23C H 0.4763 0.9543 0.8284 0.038 Uiso 1 1 calc R . . C24 C -0.1188(3) 0.92013(19) 0.90407(9) 0.0168(7) Uani 1 1 d . . . C25 C -0.1636(3) 0.90621(19) 0.94301(9) 0.0168(7) Uani 1 1 d . . . C26 C -0.2563(3) 0.9718(2) 0.95822(9) 0.0201(7) Uani 1 1 d . . . H26 H -0.2852 0.9627 0.9844 0.024 Uiso 1 1 calc R . . C27 C -0.3085(3) 1.0493(2) 0.93713(9) 0.0190(7) Uani 1 1 d . . . C28 C -0.2649(3) 1.06116(19) 0.89914(9) 0.0180(7) Uani 1 1 d . . . H28 H -0.3009 1.1138 0.8842 0.022 Uiso 1 1 calc R . . C29 C -0.1713(3) 1.00020(19) 0.88179(9) 0.0170(7) Uani 1 1 d . . . C30 C -0.1149(4) 0.8202(2) 0.96867(9) 0.0228(7) Uani 1 1 d . . . C31 C -0.1795(4) 0.8204(3) 1.00920(10) 0.0359(9) Uani 1 1 d . . . H31A H -0.1421 0.8745 1.0247 0.054 Uiso 1 1 calc R . . H31B H -0.1501 0.7632 1.0237 0.054 Uiso 1 1 calc R . . H31C H -0.2876 0.8235 1.0051 0.054 Uiso 1 1 calc R . . C32 C -0.1670(4) 0.7298(2) 0.94741(10) 0.0289(8) Uani 1 1 d . . . H32A H -0.2753 0.7272 0.9452 0.043 Uiso 1 1 calc R . . H32B H -0.1269 0.6762 0.9628 0.043 Uiso 1 1 calc R . . H32C H -0.1320 0.7284 0.9207 0.043 Uiso 1 1 calc R . . C33 C 0.0536(4) 0.8197(2) 0.97771(10) 0.0289(8) Uani 1 1 d . . . H33A H 0.1006 0.8142 0.9527 0.043 Uiso 1 1 calc R . . H33B H 0.0827 0.7668 0.9950 0.043 Uiso 1 1 calc R . . H33C H 0.0852 0.8778 0.9912 0.043 Uiso 1 1 calc R . . C34 C -0.4070(4) 1.1197(2) 0.95513(10) 0.0271(8) Uani 1 1 d . . . H34A H -0.4624 1.0891 0.9751 0.041 Uiso 1 1 calc R . . H34B H -0.4764 1.1460 0.9341 0.041 Uiso 1 1 calc R . . H34C H -0.3462 1.1697 0.9678 0.041 Uiso 1 1 calc R . . C35 C -0.1236(4) 1.0214(2) 0.83994(9) 0.0192(7) Uani 1 1 d . . . C36 C -0.1694(4) 0.9422(2) 0.81080(9) 0.0276(8) Uani 1 1 d . . . H36A H -0.1258 0.8836 0.8211 0.041 Uiso 1 1 calc R . . H36B H -0.1342 0.9558 0.7847 0.041 Uiso 1 1 calc R . . H36C H -0.2774 0.9367 0.8080 0.041 Uiso 1 1 calc R . . C37 C 0.0446(4) 1.0362(2) 0.84217(10) 0.0273(8) Uani 1 1 d . . . H37A H 0.0728 1.0857 0.8614 0.041 Uiso 1 1 calc R . . H37B H 0.0731 1.0540 0.8158 0.041 Uiso 1 1 calc R . . H37C H 0.0951 0.9783 0.8507 0.041 Uiso 1 1 calc R . . C38 C -0.1932(4) 1.1112(2) 0.82211(10) 0.0256(8) Uani 1 1 d . . . H38A H -0.3012 1.1061 0.8205 0.038 Uiso 1 1 calc R . . H38B H -0.1617 1.1207 0.7953 0.038 Uiso 1 1 calc R . . H38C H -0.1611 1.1641 0.8391 0.038 Uiso 1 1 calc R . . C39 C 0.5068(3) 0.7797(2) 0.86445(9) 0.0211(7) Uani 1 1 d . . . H39A H 0.4999 0.8116 0.8383 0.025 Uiso 1 1 calc R . . H39B H 0.6064 0.7516 0.8692 0.025 Uiso 1 1 calc R . . C40 C 0.4820(4) 0.8479(2) 0.89690(9) 0.0230(7) Uani 1 1 d . . . H40A H 0.5129 0.8201 0.9232 0.028 Uiso 1 1 calc R . . H40B H 0.5418 0.9046 0.8937 0.028 Uiso 1 1 calc R . . C41 C 0.4044(4) 0.6416(2) 0.83369(10) 0.0262(8) Uani 1 1 d . . . H41A H 0.3963 0.6729 0.8077 0.039 Uiso 1 1 calc R . . H41B H 0.3235 0.5967 0.8346 0.039 Uiso 1 1 calc R . . H41C H 0.4994 0.6089 0.8375 0.039 Uiso 1 1 calc R . . C42 C 0.3042(4) 0.9489(2) 0.92036(10) 0.0300(8) Uani 1 1 d . . . H42A H 0.3440 0.9341 0.9476 0.045 Uiso 1 1 calc R . . H42B H 0.1979 0.9613 0.9199 0.045 Uiso 1 1 calc R . . H42C H 0.3543 1.0041 0.9110 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01229(9) 0.01378(8) 0.01635(9) -0.00044(7) 0.00052(6) -0.00045(7) Si1 0.0195(5) 0.0207(4) 0.0178(5) 0.0021(3) -0.0016(4) 0.0020(4) Si2 0.0223(6) 0.0274(5) 0.0214(5) 0.0068(4) -0.0002(4) -0.0061(4) O1 0.0160(13) 0.0160(10) 0.0212(12) 0.0001(8) 0.0023(9) 0.0034(9) O2 0.0146(12) 0.0200(10) 0.0259(12) -0.0027(9) 0.0036(9) -0.0004(9) O3 0.0160(13) 0.0227(11) 0.0228(12) -0.0071(9) 0.0013(9) -0.0020(9) N1 0.0141(15) 0.0187(12) 0.0183(14) 0.0010(10) 0.0007(11) -0.0006(11) N2 0.0171(16) 0.0225(13) 0.0229(15) 0.0048(11) -0.0032(12) -0.0038(12) N3 0.0175(16) 0.0216(13) 0.0185(14) 0.0001(11) -0.0014(11) -0.0013(12) N4 0.0273(17) 0.0351(15) 0.0200(15) -0.0061(12) 0.0033(12) -0.0153(13) C1 0.0198(19) 0.0163(14) 0.0165(16) 0.0002(12) 0.0056(13) -0.0001(14) C2 0.0188(18) 0.0211(15) 0.0207(17) -0.0015(13) 0.0019(13) 0.0013(14) C3 0.018(2) 0.0280(17) 0.036(2) 0.0076(15) -0.0060(15) -0.0096(15) C4 0.023(2) 0.0334(19) 0.031(2) -0.0001(15) -0.0043(16) -0.0075(16) C5 0.039(3) 0.053(2) 0.023(2) -0.0102(17) 0.0040(17) -0.026(2) C6 0.0193(19) 0.0170(15) 0.0178(17) 0.0003(12) -0.0012(13) -0.0031(13) C7 0.026(2) 0.0276(18) 0.0277(19) -0.0037(14) 0.0035(15) -0.0022(16) C8 0.037(3) 0.0207(17) 0.046(2) -0.0057(16) -0.0004(19) 0.0013(17) C9 0.043(3) 0.0189(17) 0.039(2) 0.0072(15) -0.0129(19) -0.0121(17) C10 0.031(2) 0.0339(19) 0.0229(19) 0.0079(15) -0.0016(15) -0.0142(17) C11 0.026(2) 0.0241(16) 0.0246(19) 0.0022(14) 0.0008(15) -0.0020(15) C12 0.0230(19) 0.0201(15) 0.0183(17) 0.0009(12) -0.0007(14) -0.0047(14) C13 0.034(2) 0.0350(19) 0.030(2) -0.0090(16) -0.0044(17) 0.0064(17) C14 0.047(3) 0.0305(19) 0.035(2) 0.0006(16) -0.0189(19) 0.0034(18) C15 0.054(3) 0.0303(18) 0.0191(19) 0.0053(15) -0.0050(18) -0.0162(19) C16 0.043(2) 0.036(2) 0.0257(19) -0.0048(16) 0.0114(16) -0.0076(19) C17 0.025(2) 0.0276(17) 0.0226(17) -0.0001(14) 0.0030(14) -0.0014(15) C18 0.041(3) 0.040(2) 0.025(2) 0.0124(16) -0.0091(17) -0.0067(18) C19 0.030(2) 0.0314(18) 0.028(2) 0.0034(15) -0.0081(16) -0.0033(16) C20 0.037(3) 0.056(2) 0.034(2) -0.0069(19) -0.0041(18) 0.025(2) C21 0.043(3) 0.037(2) 0.043(2) 0.0177(17) -0.0075(19) -0.0127(19) C22 0.030(2) 0.046(2) 0.029(2) -0.0036(16) 0.0087(16) -0.0130(18) C23 0.018(2) 0.0242(17) 0.034(2) 0.0034(14) 0.0040(15) -0.0059(15) C24 0.0113(17) 0.0172(15) 0.0215(17) -0.0062(12) -0.0020(13) -0.0026(13) C25 0.0093(17) 0.0185(15) 0.0218(17) -0.0028(12) -0.0032(13) 0.0010(13) C26 0.0175(19) 0.0245(16) 0.0180(17) -0.0053(13) -0.0003(13) -0.0027(14) C27 0.0150(18) 0.0186(15) 0.0228(18) -0.0089(13) -0.0015(13) -0.0021(13) C28 0.0134(18) 0.0147(14) 0.0250(18) -0.0025(12) -0.0038(13) -0.0010(13) C29 0.0136(18) 0.0160(14) 0.0210(17) -0.0050(12) 0.0000(13) -0.0035(13) C30 0.019(2) 0.0273(17) 0.0224(18) 0.0027(13) 0.0041(14) 0.0043(15) C31 0.041(3) 0.042(2) 0.026(2) 0.0114(16) 0.0089(17) 0.0162(19) C32 0.028(2) 0.0235(16) 0.036(2) 0.0081(15) 0.0049(15) 0.0049(16) C33 0.023(2) 0.0362(19) 0.026(2) 0.0059(15) -0.0042(15) 0.0066(16) C34 0.028(2) 0.0256(17) 0.0277(19) -0.0070(14) 0.0038(15) 0.0032(16) C35 0.0178(19) 0.0195(15) 0.0209(17) 0.0003(12) 0.0049(13) -0.0002(14) C36 0.031(2) 0.0303(18) 0.0214(18) -0.0036(14) 0.0003(15) 0.0023(16) C37 0.022(2) 0.0265(17) 0.034(2) 0.0074(15) 0.0061(15) 0.0029(15) C38 0.026(2) 0.0260(17) 0.0245(19) 0.0049(14) 0.0010(15) 0.0038(15) C39 0.0119(17) 0.0273(16) 0.0238(17) 0.0031(13) 0.0001(13) -0.0028(14) C40 0.0158(19) 0.0282(17) 0.0240(18) 0.0029(14) -0.0028(14) -0.0037(14) C41 0.025(2) 0.0264(17) 0.0279(19) -0.0049(14) 0.0071(15) 0.0005(15) C42 0.034(2) 0.0272(17) 0.029(2) -0.0138(15) 0.0013(16) -0.0046(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O1 2.212(2) . ? Nd1 N4 2.422(3) . ? Nd1 N2 2.443(3) . ? Nd1 N1 2.559(2) . ? Nd1 O2 2.567(2) . ? Nd1 O3 2.609(2) . ? Nd1 N3 2.674(3) . ? Nd1 C1 2.911(3) . ? Nd1 C2 2.974(3) . ? Si1 N1 1.733(2) . ? Si1 C18 1.861(4) . ? Si1 C19 1.863(3) . ? Si1 C20 1.869(4) . ? Si2 N3 1.728(3) . ? Si2 C21 1.867(3) . ? Si2 C23 1.868(3) . ? Si2 C22 1.877(4) . ? O1 C24 1.352(4) . ? O2 C39 1.428(4) . ? O2 C41 1.434(4) . ? O3 C40 1.433(4) . ? O3 C42 1.436(4) . ? N1 C1 1.339(4) . ? N2 C1 1.307(4) . ? N2 C3 1.461(4) . ? N3 C2 1.338(4) . ? N4 C2 1.314(4) . ? N4 C5 1.461(4) . ? C1 C6 1.503(4) . ? C2 C12 1.507(4) . ? C3 C4 1.500(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.502(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C11 1.383(5) . ? C6 C7 1.384(4) . ? C7 C8 1.387(5) . ? C7 H7 0.9500 . ? C8 C9 1.370(5) . ? C8 H8 0.9500 . ? C9 C10 1.373(5) . ? C9 H9 0.9500 . ? C10 C11 1.390(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C17 1.384(5) . ? C12 C13 1.385(5) . ? C13 C14 1.382(5) . ? C13 H13 0.9500 . ? C14 C15 1.365(5) . ? C14 H14 0.9500 . ? C15 C16 1.374(5) . ? C15 H15 0.9500 . ? C16 C17 1.395(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? 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 C25 1.420(4) . ? C24 C29 1.431(4) . ? C25 C26 1.391(4) . ? C25 C30 1.549(4) . ? C26 C27 1.382(4) . ? C26 H26 0.9500 . ? C27 C28 1.382(4) . ? C27 C34 1.512(4) . ? C28 C29 1.385(4) . ? C28 H28 0.9500 . ? C29 C35 1.541(4) . ? C30 C31 1.532(5) . ? C30 C33 1.532(5) . ? C30 C32 1.536(4) . ? 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 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.534(4) . ? C35 C38 1.535(4) . ? C35 C37 1.537(5) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.499(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 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 O1 Nd1 N4 110.06(9) . . ? O1 Nd1 N2 94.79(9) . . ? N4 Nd1 N2 70.14(9) . . ? O1 Nd1 N1 109.74(8) . . ? N4 Nd1 N1 111.85(8) . . ? N2 Nd1 N1 53.57(8) . . ? O1 Nd1 O2 142.66(7) . . ? N4 Nd1 O2 103.54(8) . . ? N2 Nd1 O2 111.88(7) . . ? N1 Nd1 O2 70.65(7) . . ? O1 Nd1 O3 82.93(7) . . ? N4 Nd1 O3 136.60(8) . . ? N2 Nd1 O3 152.24(7) . . ? N1 Nd1 O3 101.06(7) . . ? O2 Nd1 O3 61.18(6) . . ? O1 Nd1 N3 109.68(7) . . ? N4 Nd1 N3 52.33(8) . . ? N2 Nd1 N3 122.01(8) . . ? N1 Nd1 N3 140.58(8) . . ? O2 Nd1 N3 78.51(7) . . ? O3 Nd1 N3 84.28(7) . . ? O1 Nd1 C1 106.08(8) . . ? N4 Nd1 C1 89.03(9) . . ? N2 Nd1 C1 26.45(8) . . ? N1 Nd1 C1 27.37(8) . . ? O2 Nd1 C1 90.02(8) . . ? O3 Nd1 C1 128.22(7) . . ? N3 Nd1 C1 134.20(8) . . ? O1 Nd1 C2 110.79(8) . . ? N4 Nd1 C2 25.67(8) . . ? N2 Nd1 C2 95.74(8) . . ? N1 Nd1 C2 130.47(8) . . ? O2 Nd1 C2 92.65(8) . . ? O3 Nd1 C2 110.99(8) . . ? N3 Nd1 C2 26.74(8) . . ? C1 Nd1 C2 112.50(8) . . ? N1 Si1 C18 114.42(15) . . ? N1 Si1 C19 107.79(13) . . ? C18 Si1 C19 106.95(16) . . ? N1 Si1 C20 113.97(15) . . ? C18 Si1 C20 107.05(18) . . ? C19 Si1 C20 106.14(18) . . ? N3 Si2 C21 115.30(16) . . ? N3 Si2 C23 109.56(14) . . ? C21 Si2 C23 104.90(16) . . ? N3 Si2 C22 112.69(15) . . ? C21 Si2 C22 106.49(18) . . ? C23 Si2 C22 107.33(16) . . ? C24 O1 Nd1 179.4(2) . . ? C39 O2 C41 113.1(2) . . ? C39 O2 Nd1 118.12(17) . . ? C41 O2 Nd1 106.41(18) . . ? C40 O3 C42 110.5(2) . . ? C40 O3 Nd1 121.87(16) . . ? C42 O3 Nd1 125.95(19) . . ? C1 N1 Si1 127.7(2) . . ? C1 N1 Nd1 91.11(17) . . ? Si1 N1 Nd1 140.64(13) . . ? C1 N2 C3 121.2(2) . . ? C1 N2 Nd1 97.17(19) . . ? C3 N2 Nd1 138.60(19) . . ? C2 N3 Si2 125.1(2) . . ? C2 N3 Nd1 89.24(18) . . ? Si2 N3 Nd1 145.46(13) . . ? C2 N4 C5 121.6(3) . . ? C2 N4 Nd1 101.37(19) . . ? C5 N4 Nd1 136.7(2) . . ? N2 C1 N1 117.1(3) . . ? N2 C1 C6 120.2(3) . . ? N1 C1 C6 122.7(3) . . ? N2 C1 Nd1 56.38(15) . . ? N1 C1 Nd1 61.52(14) . . ? C6 C1 Nd1 171.0(2) . . ? N4 C2 N3 116.7(3) . . ? N4 C2 C12 120.1(3) . . ? N3 C2 C12 123.2(3) . . ? N4 C2 Nd1 52.96(15) . . ? N3 C2 Nd1 64.02(16) . . ? C12 C2 Nd1 171.3(2) . . ? N2 C3 C4 111.3(3) . . ? N2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 114.6(3) . . ? C3 C4 H4A 108.6 . . ? C5 C4 H4A 108.6 . . ? C3 C4 H4B 108.6 . . ? C5 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? N4 C5 C4 111.4(3) . . ? N4 C5 H5A 109.3 . . ? C4 C5 H5A 109.3 . . ? N4 C5 H5B 109.3 . . ? C4 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C11 C6 C7 119.4(3) . . ? C11 C6 C1 119.1(3) . . ? C7 C6 C1 121.5(3) . . ? C6 C7 C8 119.8(3) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 120.8(3) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 119.6(3) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C11 120.4(3) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C6 C11 C10 120.0(3) . . ? C6 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C17 C12 C13 118.3(3) . . ? C17 C12 C2 120.6(3) . . ? C13 C12 C2 121.1(3) . . ? C14 C13 C12 120.9(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 120.5(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.7(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 120.2(3) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C12 C17 C16 120.5(3) . . ? C12 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O1 C24 C25 120.9(3) . . ? O1 C24 C29 120.0(3) . . ? C25 C24 C29 119.1(3) . . ? C26 C25 C24 118.5(3) . . ? C26 C25 C30 119.1(3) . . ? C24 C25 C30 122.4(3) . . ? C27 C26 C25 123.2(3) . . ? C27 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? C28 C27 C26 117.4(3) . . ? C28 C27 C34 121.1(3) . . ? C26 C27 C34 121.4(3) . . ? C27 C28 C29 123.3(3) . . ? C27 C28 H28 118.3 . . ? C29 C28 H28 118.3 . . ? C28 C29 C24 118.4(3) . . ? C28 C29 C35 119.6(3) . . ? C24 C29 C35 122.0(3) . . ? C31 C30 C33 106.1(3) . . ? C31 C30 C32 106.8(3) . . ? C33 C30 C32 110.4(3) . . ? C31 C30 C25 112.5(3) . . ? C33 C30 C25 110.2(3) . . ? C32 C30 C25 110.7(2) . . ? 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 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C27 C34 H34A 109.5 . . ? C27 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C27 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C38 107.1(2) . . ? C36 C35 C37 110.2(3) . . ? C38 C35 C37 106.0(3) . . ? C36 C35 C29 110.8(2) . . ? C38 C35 C29 112.5(3) . . ? C37 C35 C29 110.0(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O2 C39 C40 107.8(3) . . ? O2 C39 H39A 110.1 . . ? C40 C39 H39A 110.1 . . ? O2 C39 H39B 110.1 . . ? C40 C39 H39B 110.1 . . ? H39A C39 H39B 108.5 . . ? O3 C40 C39 109.0(2) . . ? O3 C40 H40A 109.9 . . ? C39 C40 H40A 109.9 . . ? O3 C40 H40B 109.9 . . ? C39 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? O2 C41 H41A 109.5 . . ? O2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O3 C42 H42A 109.5 . . ? O3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 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 N4 Nd1 O1 C24 11(24) . . . . ? N2 Nd1 O1 C24 -60(24) . . . . ? N1 Nd1 O1 C24 -113(23) . . . . ? O2 Nd1 O1 C24 164(100) . . . . ? O3 Nd1 O1 C24 148(76) . . . . ? N3 Nd1 O1 C24 67(24) . . . . ? C1 Nd1 O1 C24 -84(24) . . . . ? C2 Nd1 O1 C24 38(24) . . . . ? O1 Nd1 O2 C39 -46.7(2) . . . . ? N4 Nd1 O2 C39 107.14(19) . . . . ? N2 Nd1 O2 C39 -179.12(18) . . . . ? N1 Nd1 O2 C39 -144.1(2) . . . . ? O3 Nd1 O2 C39 -28.95(18) . . . . ? N3 Nd1 O2 C39 60.80(19) . . . . ? C1 Nd1 O2 C39 -163.86(19) . . . . ? C2 Nd1 O2 C39 83.62(19) . . . . ? O1 Nd1 O2 C41 -175.00(17) . . . . ? N4 Nd1 O2 C41 -21.20(19) . . . . ? N2 Nd1 O2 C41 52.54(19) . . . . ? N1 Nd1 O2 C41 87.53(18) . . . . ? O3 Nd1 O2 C41 -157.29(19) . . . . ? N3 Nd1 O2 C41 -67.54(18) . . . . ? C1 Nd1 O2 C41 67.80(18) . . . . ? C2 Nd1 O2 C41 -44.72(18) . . . . ? O1 Nd1 O3 C40 170.0(2) . . . . ? N4 Nd1 O3 C40 -78.2(2) . . . . ? N2 Nd1 O3 C40 83.1(3) . . . . ? N1 Nd1 O3 C40 61.2(2) . . . . ? O2 Nd1 O3 C40 0.69(19) . . . . ? N3 Nd1 O3 C40 -79.3(2) . . . . ? C1 Nd1 O3 C40 65.0(2) . . . . ? C2 Nd1 O3 C40 -80.4(2) . . . . ? O1 Nd1 O3 C42 6.0(2) . . . . ? N4 Nd1 O3 C42 117.8(2) . . . . ? N2 Nd1 O3 C42 -80.9(3) . . . . ? N1 Nd1 O3 C42 -102.9(2) . . . . ? O2 Nd1 O3 C42 -163.3(2) . . . . ? N3 Nd1 O3 C42 116.7(2) . . . . ? C1 Nd1 O3 C42 -99.0(2) . . . . ? C2 Nd1 O3 C42 115.6(2) . . . . ? C18 Si1 N1 C1 -38.3(3) . . . . ? C19 Si1 N1 C1 -157.1(3) . . . . ? C20 Si1 N1 C1 85.4(3) . . . . ? C18 Si1 N1 Nd1 152.5(2) . . . . ? C19 Si1 N1 Nd1 33.6(3) . . . . ? C20 Si1 N1 Nd1 -83.9(2) . . . . ? O1 Nd1 N1 C1 86.95(18) . . . . ? N4 Nd1 N1 C1 -35.5(2) . . . . ? N2 Nd1 N1 C1 5.84(17) . . . . ? O2 Nd1 N1 C1 -132.76(19) . . . . ? O3 Nd1 N1 C1 173.34(17) . . . . ? N3 Nd1 N1 C1 -92.2(2) . . . . ? C2 Nd1 N1 C1 -56.4(2) . . . . ? O1 Nd1 N1 Si1 -101.5(2) . . . . ? N4 Nd1 N1 Si1 136.0(2) . . . . ? N2 Nd1 N1 Si1 177.4(3) . . . . ? O2 Nd1 N1 Si1 38.8(2) . . . . ? O3 Nd1 N1 Si1 -15.1(2) . . . . ? N3 Nd1 N1 Si1 79.3(2) . . . . ? C1 Nd1 N1 Si1 171.5(3) . . . . ? C2 Nd1 N1 Si1 115.2(2) . . . . ? O1 Nd1 N2 C1 -117.09(19) . . . . ? N4 Nd1 N2 C1 133.3(2) . . . . ? N1 Nd1 N2 C1 -6.03(17) . . . . ? O2 Nd1 N2 C1 36.2(2) . . . . ? O3 Nd1 N2 C1 -33.2(3) . . . . ? N3 Nd1 N2 C1 126.10(18) . . . . ? C2 Nd1 N2 C1 131.41(19) . . . . ? O1 Nd1 N2 C3 84.1(3) . . . . ? N4 Nd1 N2 C3 -25.5(3) . . . . ? N1 Nd1 N2 C3 -164.9(4) . . . . ? O2 Nd1 N2 C3 -122.6(3) . . . . ? O3 Nd1 N2 C3 168.0(3) . . . . ? N3 Nd1 N2 C3 -32.7(4) . . . . ? C1 Nd1 N2 C3 -158.8(4) . . . . ? C2 Nd1 N2 C3 -27.4(3) . . . . ? C21 Si2 N3 C2 44.4(3) . . . . ? C23 Si2 N3 C2 162.5(3) . . . . ? C22 Si2 N3 C2 -78.1(3) . . . . ? C21 Si2 N3 Nd1 -128.0(2) . . . . ? C23 Si2 N3 Nd1 -10.0(3) . . . . ? C22 Si2 N3 Nd1 109.5(2) . . . . ? O1 Nd1 N3 C2 -97.36(17) . . . . ? N4 Nd1 N3 C2 3.25(17) . . . . ? N2 Nd1 N3 C2 11.8(2) . . . . ? N1 Nd1 N3 C2 81.8(2) . . . . ? O2 Nd1 N3 C2 120.55(18) . . . . ? O3 Nd1 N3 C2 -177.74(18) . . . . ? C1 Nd1 N3 C2 41.9(2) . . . . ? O1 Nd1 N3 Si2 76.4(2) . . . . ? N4 Nd1 N3 Si2 177.0(3) . . . . ? N2 Nd1 N3 Si2 -174.4(2) . . . . ? N1 Nd1 N3 Si2 -104.4(2) . . . . ? O2 Nd1 N3 Si2 -65.6(2) . . . . ? O3 Nd1 N3 Si2 -3.9(2) . . . . ? C1 Nd1 N3 Si2 -144.3(2) . . . . ? C2 Nd1 N3 Si2 173.8(4) . . . . ? O1 Nd1 N4 C2 96.5(2) . . . . ? N2 Nd1 N4 C2 -175.7(2) . . . . ? N1 Nd1 N4 C2 -141.3(2) . . . . ? O2 Nd1 N4 C2 -67.0(2) . . . . ? O3 Nd1 N4 C2 -4.8(3) . . . . ? N3 Nd1 N4 C2 -3.37(18) . . . . ? C1 Nd1 N4 C2 -156.7(2) . . . . ? O1 Nd1 N4 C5 -76.6(4) . . . . ? N2 Nd1 N4 C5 11.3(3) . . . . ? N1 Nd1 N4 C5 45.7(4) . . . . ? O2 Nd1 N4 C5 120.0(3) . . . . ? O3 Nd1 N4 C5 -177.9(3) . . . . ? N3 Nd1 N4 C5 -176.5(4) . . . . ? C1 Nd1 N4 C5 30.2(3) . . . . ? C2 Nd1 N4 C5 -173.1(5) . . . . ? C3 N2 C1 N1 174.2(3) . . . . ? Nd1 N2 C1 N1 10.5(3) . . . . ? C3 N2 C1 C6 -6.4(5) . . . . ? Nd1 N2 C1 C6 -170.1(2) . . . . ? C3 N2 C1 Nd1 163.8(3) . . . . ? Si1 N1 C1 N2 176.9(2) . . . . ? Nd1 N1 C1 N2 -9.9(3) . . . . ? Si1 N1 C1 C6 -2.5(4) . . . . ? Nd1 N1 C1 C6 170.7(3) . . . . ? Si1 N1 C1 Nd1 -173.2(3) . . . . ? O1 Nd1 C1 N2 67.4(2) . . . . ? N4 Nd1 C1 N2 -43.2(2) . . . . ? N1 Nd1 C1 N2 169.4(3) . . . . ? O2 Nd1 C1 N2 -146.75(19) . . . . ? O3 Nd1 C1 N2 161.08(17) . . . . ? N3 Nd1 C1 N2 -72.9(2) . . . . ? C2 Nd1 C1 N2 -53.9(2) . . . . ? O1 Nd1 C1 N1 -102.00(18) . . . . ? N4 Nd1 C1 N1 147.39(18) . . . . ? N2 Nd1 C1 N1 -169.4(3) . . . . ? O2 Nd1 C1 N1 43.85(18) . . . . ? O3 Nd1 C1 N1 -8.3(2) . . . . ? N3 Nd1 C1 N1 117.73(18) . . . . ? C2 Nd1 C1 N1 136.72(17) . . . . ? O1 Nd1 C1 C6 137.7(14) . . . . ? N4 Nd1 C1 C6 27.1(14) . . . . ? N2 Nd1 C1 C6 70.3(14) . . . . ? N1 Nd1 C1 C6 -120.3(15) . . . . ? O2 Nd1 C1 C6 -76.4(14) . . . . ? O3 Nd1 C1 C6 -128.6(14) . . . . ? N3 Nd1 C1 C6 -2.6(15) . . . . ? C2 Nd1 C1 C6 16.4(14) . . . . ? C5 N4 C2 N3 -179.6(3) . . . . ? Nd1 N4 C2 N3 6.0(3) . . . . ? C5 N4 C2 C12 0.7(5) . . . . ? Nd1 N4 C2 C12 -173.7(2) . . . . ? C5 N4 C2 Nd1 174.4(4) . . . . ? Si2 N3 C2 N4 179.0(2) . . . . ? Nd1 N3 C2 N4 -5.3(3) . . . . ? Si2 N3 C2 C12 -1.3(4) . . . . ? Nd1 N3 C2 C12 174.4(3) . . . . ? Si2 N3 C2 Nd1 -175.7(2) . . . . ? O1 Nd1 C2 N4 -93.3(2) . . . . ? N2 Nd1 C2 N4 4.1(2) . . . . ? N1 Nd1 C2 N4 49.8(2) . . . . ? O2 Nd1 C2 N4 116.4(2) . . . . ? O3 Nd1 C2 N4 176.5(2) . . . . ? N3 Nd1 C2 N4 174.1(3) . . . . ? C1 Nd1 C2 N4 25.3(2) . . . . ? O1 Nd1 C2 N3 92.68(18) . . . . ? N4 Nd1 C2 N3 -174.1(3) . . . . ? N2 Nd1 C2 N3 -169.96(17) . . . . ? N1 Nd1 C2 N3 -124.28(17) . . . . ? O2 Nd1 C2 N3 -57.65(17) . . . . ? O3 Nd1 C2 N3 2.41(19) . . . . ? C1 Nd1 C2 N3 -148.76(16) . . . . ? O1 Nd1 C2 C12 -54.5(13) . . . . ? N4 Nd1 C2 C12 38.7(13) . . . . ? N2 Nd1 C2 C12 42.8(13) . . . . ? N1 Nd1 C2 C12 88.5(13) . . . . ? O2 Nd1 C2 C12 155.1(13) . . . . ? O3 Nd1 C2 C12 -144.8(13) . . . . ? N3 Nd1 C2 C12 -147.2(14) . . . . ? C1 Nd1 C2 C12 64.0(13) . . . . ? C1 N2 C3 C4 -157.0(3) . . . . ? Nd1 N2 C3 C4 -1.8(5) . . . . ? N2 C3 C4 C5 58.2(4) . . . . ? C2 N4 C5 C4 -145.4(3) . . . . ? Nd1 N4 C5 C4 26.7(5) . . . . ? C3 C4 C5 N4 -70.2(4) . . . . ? N2 C1 C6 C11 -73.8(4) . . . . ? N1 C1 C6 C11 105.5(4) . . . . ? Nd1 C1 C6 C11 -138.9(13) . . . . ? N2 C1 C6 C7 105.2(4) . . . . ? N1 C1 C6 C7 -75.4(4) . . . . ? Nd1 C1 C6 C7 40.1(16) . . . . ? C11 C6 C7 C8 -1.0(5) . . . . ? C1 C6 C7 C8 -180.0(3) . . . . ? C6 C7 C8 C9 -0.3(5) . . . . ? C7 C8 C9 C10 0.8(5) . . . . ? C8 C9 C10 C11 -0.1(5) . . . . ? C7 C6 C11 C10 1.6(5) . . . . ? C1 C6 C11 C10 -179.3(3) . . . . ? C9 C10 C11 C6 -1.1(5) . . . . ? N4 C2 C12 C17 -98.9(4) . . . . ? N3 C2 C12 C17 81.4(4) . . . . ? Nd1 C2 C12 C17 -134.1(12) . . . . ? N4 C2 C12 C13 78.6(4) . . . . ? N3 C2 C12 C13 -101.1(4) . . . . ? Nd1 C2 C12 C13 43.4(15) . . . . ? C17 C12 C13 C14 -1.4(5) . . . . ? C2 C12 C13 C14 -179.0(3) . . . . ? C12 C13 C14 C15 1.1(5) . . . . ? C13 C14 C15 C16 0.3(5) . . . . ? C14 C15 C16 C17 -1.2(5) . . . . ? C13 C12 C17 C16 0.5(5) . . . . ? C2 C12 C17 C16 178.1(3) . . . . ? C15 C16 C17 C12 0.8(5) . . . . ? Nd1 O1 C24 C25 122(23) . . . . ? Nd1 O1 C24 C29 -60(24) . . . . ? O1 C24 C25 C26 178.4(3) . . . . ? C29 C24 C25 C26 -0.6(4) . . . . ? O1 C24 C25 C30 -2.6(4) . . . . ? C29 C24 C25 C30 178.5(3) . . . . ? C24 C25 C26 C27 0.7(5) . . . . ? C30 C25 C26 C27 -178.3(3) . . . . ? C25 C26 C27 C28 -0.1(5) . . . . ? C25 C26 C27 C34 -178.9(3) . . . . ? C26 C27 C28 C29 -0.8(5) . . . . ? C34 C27 C28 C29 178.0(3) . . . . ? C27 C28 C29 C24 1.0(4) . . . . ? C27 C28 C29 C35 -177.4(3) . . . . ? O1 C24 C29 C28 -179.2(3) . . . . ? C25 C24 C29 C28 -0.3(4) . . . . ? O1 C24 C29 C35 -0.9(4) . . . . ? C25 C24 C29 C35 178.1(3) . . . . ? C26 C25 C30 C31 -0.1(4) . . . . ? C24 C25 C30 C31 -179.1(3) . . . . ? C26 C25 C30 C33 -118.3(3) . . . . ? C24 C25 C30 C33 62.7(4) . . . . ? C26 C25 C30 C32 119.3(3) . . . . ? C24 C25 C30 C32 -59.7(4) . . . . ? C28 C29 C35 C36 -121.2(3) . . . . ? C24 C29 C35 C36 60.5(4) . . . . ? C28 C29 C35 C38 -1.2(4) . . . . ? C24 C29 C35 C38 -179.6(3) . . . . ? C28 C29 C35 C37 116.7(3) . . . . ? C24 C29 C35 C37 -61.6(4) . . . . ? C41 O2 C39 C40 177.6(2) . . . . ? Nd1 O2 C39 C40 52.4(3) . . . . ? C42 O3 C40 C39 -169.5(3) . . . . ? Nd1 O3 C40 C39 24.3(3) . . . . ? O2 C39 C40 O3 -46.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.612 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.082 data_complex5 _database_code_depnum_ccdc_archive 'CCDC 915747' #TrackingRef '915747.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H67 N4 O3 Si2 Sm' _chemical_formula_sum 'C42 H67 N4 O3 Si2 Sm' _chemical_formula_weight 882.53 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 9.0917(4) _cell_length_b 14.3482(7) _cell_length_c 33.7910(17) _cell_angle_alpha 90.00 _cell_angle_beta 95.344(2) _cell_angle_gamma 90.00 _cell_volume 4388.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9972 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 31.19 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_absorpt_coefficient_mu 1.433 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4337 _exptl_absorpt_correction_T_max 0.7626 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 131137 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_unetI/netI 0.0167 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8156 _reflns_number_gt 7494 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+4.6085P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8156 _refine_ls_number_parameters 484 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0620 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.122042(13) 0.761106(8) 0.861986(3) 0.01794(5) Uani 1 1 d . . . Si1 Si 0.28896(8) 0.57081(5) 0.94203(2) 0.02553(15) Uani 1 1 d . . . Si2 Si 0.31504(9) 0.90980(6) 0.77304(2) 0.03184(17) Uani 1 1 d . . . O1 O -0.02589(18) 0.85894(11) 0.88826(5) 0.0233(4) Uani 1 1 d . . . O2 O 0.38946(19) 0.70925(12) 0.86365(5) 0.0275(4) Uani 1 1 d . . . O3 O 0.32370(19) 0.87017(12) 0.89484(5) 0.0271(4) Uani 1 1 d . . . N1 N 0.1613(2) 0.61939(14) 0.90683(6) 0.0232(4) Uani 1 1 d . . . N2 N -0.0449(2) 0.63079(15) 0.86438(7) 0.0284(5) Uani 1 1 d . . . N3 N 0.2026(2) 0.83054(15) 0.79454(6) 0.0253(5) Uani 1 1 d . . . N4 N 0.0264(3) 0.72042(18) 0.79566(7) 0.0364(6) Uani 1 1 d . . . C1 C 0.0409(3) 0.57886(16) 0.88866(7) 0.0220(5) Uani 1 1 d . . . C2 C 0.0987(3) 0.77887(18) 0.77476(7) 0.0257(5) Uani 1 1 d . . . C3 C -0.1708(3) 0.5913(2) 0.84024(9) 0.0353(7) Uani 1 1 d . . . H3A H -0.2570 0.5891 0.8561 0.042 Uiso 1 1 calc R . . H3B H -0.1473 0.5266 0.8328 0.042 Uiso 1 1 calc R . . C4 C -0.2099(4) 0.6468(2) 0.80348(9) 0.0453(8) Uani 1 1 d . . . H4A H -0.2938 0.6159 0.7879 0.054 Uiso 1 1 calc R . . H4B H -0.2440 0.7090 0.8113 0.054 Uiso 1 1 calc R . . C5 C -0.0891(4) 0.6595(3) 0.77738(9) 0.0503(9) Uani 1 1 d . . . H5A H -0.0460 0.5980 0.7718 0.060 Uiso 1 1 calc R . . H5B H -0.1300 0.6867 0.7517 0.060 Uiso 1 1 calc R . . C6 C 0.0018(3) 0.47847(17) 0.89520(7) 0.0251(5) Uani 1 1 d . . . C7 C 0.0763(3) 0.40659(19) 0.87857(9) 0.0365(7) Uani 1 1 d . . . H7 H 0.1541 0.4198 0.8625 0.044 Uiso 1 1 calc R . . C8 C 0.0367(4) 0.3149(2) 0.88546(11) 0.0488(8) Uani 1 1 d . . . H8 H 0.0877 0.2655 0.8739 0.059 Uiso 1 1 calc R . . C9 C -0.0747(4) 0.2948(2) 0.90867(10) 0.0471(8) Uani 1 1 d . . . H9 H -0.0997 0.2318 0.9136 0.056 Uiso 1 1 calc R . . C10 C -0.1501(4) 0.3659(2) 0.92482(9) 0.0411(7) Uani 1 1 d . . . H10 H -0.2281 0.3521 0.9408 0.049 Uiso 1 1 calc R . . C11 C -0.1130(3) 0.4576(2) 0.91797(8) 0.0323(6) Uani 1 1 d . . . H11 H -0.1665 0.5066 0.9290 0.039 Uiso 1 1 calc R . . C12 C 0.0620(3) 0.78547(19) 0.73021(8) 0.0284(6) Uani 1 1 d . . . C13 C -0.0603(4) 0.8342(2) 0.71422(9) 0.0443(8) Uani 1 1 d . . . H13 H -0.1219 0.8647 0.7314 0.053 Uiso 1 1 calc R . . C14 C -0.0945(4) 0.8392(2) 0.67349(10) 0.0532(9) Uani 1 1 d . . . H14 H -0.1779 0.8740 0.6629 0.064 Uiso 1 1 calc R . . C15 C -0.0081(4) 0.7940(2) 0.64850(9) 0.0500(9) Uani 1 1 d . . . H15 H -0.0313 0.7976 0.6205 0.060 Uiso 1 1 calc R . . C16 C 0.1110(4) 0.7438(2) 0.66374(10) 0.0474(8) Uani 1 1 d . . . H16 H 0.1699 0.7117 0.6463 0.057 Uiso 1 1 calc R . . C17 C 0.1474(3) 0.7390(2) 0.70466(9) 0.0358(7) Uani 1 1 d . . . H17 H 0.2308 0.7039 0.7150 0.043 Uiso 1 1 calc R . . C18 C 0.2082(4) 0.4930(2) 0.97830(9) 0.0474(8) Uani 1 1 d . . . H18A H 0.1247 0.5244 0.9890 0.071 Uiso 1 1 calc R . . H18B H 0.2835 0.4783 1.0001 0.071 Uiso 1 1 calc R . . H18C H 0.1739 0.4353 0.9650 0.071 Uiso 1 1 calc R . . C19 C 0.3825(3) 0.6677(2) 0.97111(9) 0.0403(7) Uani 1 1 d . . . H19A H 0.4192 0.7134 0.9529 0.060 Uiso 1 1 calc R . . H19B H 0.4655 0.6428 0.9885 0.060 Uiso 1 1 calc R . . H19C H 0.3120 0.6978 0.9873 0.060 Uiso 1 1 calc R . . C20 C 0.4378(4) 0.5033(3) 0.92029(10) 0.0579(10) Uani 1 1 d . . . H20A H 0.3932 0.4544 0.9028 0.087 Uiso 1 1 calc R . . H20B H 0.5027 0.4749 0.9417 0.087 Uiso 1 1 calc R . . H20C H 0.4956 0.5453 0.9049 0.087 Uiso 1 1 calc R . . C21 C 0.2174(4) 0.9880(2) 0.73512(11) 0.0553(10) Uani 1 1 d . . . H21A H 0.1870 0.9521 0.7111 0.083 Uiso 1 1 calc R . . H21B H 0.2839 1.0383 0.7286 0.083 Uiso 1 1 calc R . . H21C H 0.1300 1.0146 0.7458 0.083 Uiso 1 1 calc R . . C22 C 0.4681(4) 0.8520(3) 0.74846(10) 0.0481(8) Uani 1 1 d . . . H22A H 0.5192 0.8075 0.7669 0.072 Uiso 1 1 calc R . . H22B H 0.5382 0.8994 0.7410 0.072 Uiso 1 1 calc R . . H22C H 0.4266 0.8191 0.7246 0.072 Uiso 1 1 calc R . . C23 C 0.4024(3) 0.9894(2) 0.81204(9) 0.0359(7) Uani 1 1 d . . . H23A H 0.3272 1.0117 0.8288 0.054 Uiso 1 1 calc R . . H23B H 0.4464 1.0427 0.7994 0.054 Uiso 1 1 calc R . . H23C H 0.4793 0.9557 0.8285 0.054 Uiso 1 1 calc R . . C24 C -0.1181(3) 0.91952(16) 0.90371(7) 0.0209(5) Uani 1 1 d . . . C25 C -0.1637(3) 0.90509(17) 0.94266(7) 0.0228(5) Uani 1 1 d . . . C26 C -0.2562(3) 0.97150(18) 0.95757(8) 0.0262(5) Uani 1 1 d . . . H26 H -0.2850 0.9627 0.9836 0.031 Uiso 1 1 calc R . . C27 C -0.3081(3) 1.04919(17) 0.93664(8) 0.0258(5) Uani 1 1 d . . . C28 C -0.2651(3) 1.06086(17) 0.89874(8) 0.0246(5) Uani 1 1 d . . . H28 H -0.3017 1.1132 0.8837 0.030 Uiso 1 1 calc R . . C29 C -0.1706(3) 0.99933(16) 0.88170(7) 0.0220(5) Uani 1 1 d . . . C30 C -0.1155(3) 0.81963(19) 0.96826(8) 0.0304(6) Uani 1 1 d . . . C31 C -0.1810(4) 0.8201(2) 1.00864(9) 0.0485(8) Uani 1 1 d . . . H31A H -0.1445 0.8747 1.0240 0.073 Uiso 1 1 calc R . . H31B H -0.1511 0.7633 1.0233 0.073 Uiso 1 1 calc R . . H31C H -0.2890 0.8227 1.0043 0.073 Uiso 1 1 calc R . . C32 C -0.1687(3) 0.72933(19) 0.94720(9) 0.0358(7) Uani 1 1 d . . . H32A H -0.2769 0.7267 0.9454 0.054 Uiso 1 1 calc R . . H32B H -0.1277 0.6756 0.9624 0.054 Uiso 1 1 calc R . . H32C H -0.1356 0.7280 0.9204 0.054 Uiso 1 1 calc R . . C33 C 0.0525(3) 0.8178(2) 0.97719(9) 0.0402(7) Uani 1 1 d . . . H33A H 0.0988 0.8120 0.9523 0.060 Uiso 1 1 calc R . . H33B H 0.0808 0.7646 0.9944 0.060 Uiso 1 1 calc R . . H33C H 0.0854 0.8757 0.9906 0.060 Uiso 1 1 calc R . . C34 C -0.4067(3) 1.1194(2) 0.95427(9) 0.0357(7) Uani 1 1 d . . . H34A H -0.4585 1.0895 0.9750 0.054 Uiso 1 1 calc R . . H34B H -0.4791 1.1432 0.9334 0.054 Uiso 1 1 calc R . . H34C H -0.3468 1.1711 0.9658 0.054 Uiso 1 1 calc R . . C35 C -0.1237(3) 1.02086(18) 0.84014(8) 0.0259(5) Uani 1 1 d . . . C36 C -0.1697(3) 0.9420(2) 0.81115(8) 0.0368(7) Uani 1 1 d . . . H36A H -0.1263 0.8832 0.8214 0.055 Uiso 1 1 calc R . . H36B H -0.1348 0.9556 0.7852 0.055 Uiso 1 1 calc R . . H36C H -0.2776 0.9365 0.8083 0.055 Uiso 1 1 calc R . . C37 C 0.0441(3) 1.0361(2) 0.84254(9) 0.0361(7) Uani 1 1 d . . . H37A H 0.0725 1.0841 0.8624 0.054 Uiso 1 1 calc R . . H37B H 0.0720 1.0564 0.8166 0.054 Uiso 1 1 calc R . . H37C H 0.0949 0.9777 0.8501 0.054 Uiso 1 1 calc R . . C38 C -0.1939(3) 1.1107(2) 0.82222(9) 0.0349(6) Uani 1 1 d . . . H38A H -0.3018 1.1048 0.8201 0.052 Uiso 1 1 calc R . . H38B H -0.1610 1.1208 0.7958 0.052 Uiso 1 1 calc R . . H38C H -0.1638 1.1636 0.8394 0.052 Uiso 1 1 calc R . . C39 C 0.5012(3) 0.7789(2) 0.86406(9) 0.0319(6) Uani 1 1 d . . . H39A H 0.4951 0.8117 0.8382 0.038 Uiso 1 1 calc R . . H39B H 0.6002 0.7499 0.8687 0.038 Uiso 1 1 calc R . . C40 C 0.4774(3) 0.84641(19) 0.89686(8) 0.0304(6) Uani 1 1 d . . . H40A H 0.5089 0.8179 0.9229 0.037 Uiso 1 1 calc R . . H40B H 0.5371 0.9033 0.8939 0.037 Uiso 1 1 calc R . . C41 C 0.4003(3) 0.6415(2) 0.83314(9) 0.0363(7) Uani 1 1 d . . . H41A H 0.3919 0.6725 0.8072 0.054 Uiso 1 1 calc R . . H41B H 0.3206 0.5958 0.8340 0.054 Uiso 1 1 calc R . . H41C H 0.4960 0.6098 0.8373 0.054 Uiso 1 1 calc R . . C42 C 0.3008(3) 0.9470(2) 0.92074(9) 0.0379(7) Uani 1 1 d . . . H42A H 0.3428 0.9320 0.9478 0.057 Uiso 1 1 calc R . . H42B H 0.1947 0.9588 0.9208 0.057 Uiso 1 1 calc R . . H42C H 0.3494 1.0027 0.9113 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01602(7) 0.01761(7) 0.01986(7) -0.00068(5) -0.00004(5) -0.00076(5) Si1 0.0258(4) 0.0271(4) 0.0229(4) 0.0031(3) -0.0018(3) 0.0024(3) Si2 0.0305(4) 0.0357(4) 0.0288(4) 0.0092(3) -0.0002(3) -0.0086(3) O1 0.0209(9) 0.0219(9) 0.0275(9) -0.0002(7) 0.0043(7) 0.0038(7) O2 0.0211(9) 0.0284(9) 0.0333(10) -0.0038(8) 0.0040(8) -0.0006(7) O3 0.0220(9) 0.0303(10) 0.0283(10) -0.0068(8) -0.0021(7) -0.0043(7) N1 0.0211(11) 0.0228(10) 0.0253(11) 0.0017(8) -0.0004(9) -0.0018(8) N2 0.0254(12) 0.0275(11) 0.0307(12) 0.0059(9) -0.0058(9) -0.0057(9) N3 0.0221(11) 0.0309(11) 0.0222(11) 0.0022(9) -0.0018(9) -0.0043(9) N4 0.0381(14) 0.0477(14) 0.0236(12) -0.0053(10) 0.0038(10) -0.0213(12) C1 0.0237(13) 0.0205(12) 0.0225(12) 0.0013(10) 0.0058(10) -0.0018(10) C2 0.0257(13) 0.0303(13) 0.0209(13) -0.0007(10) 0.0009(10) 0.0003(11) C3 0.0266(15) 0.0364(15) 0.0408(17) 0.0089(13) -0.0085(12) -0.0132(12) C4 0.0401(18) 0.055(2) 0.0390(17) 0.0024(15) -0.0058(14) -0.0149(15) C5 0.051(2) 0.071(2) 0.0294(16) -0.0165(15) 0.0061(14) -0.0364(18) C6 0.0279(14) 0.0229(12) 0.0236(13) 0.0010(10) -0.0023(10) -0.0044(10) C7 0.0358(16) 0.0294(15) 0.0448(17) -0.0042(12) 0.0055(13) -0.0031(12) C8 0.055(2) 0.0262(15) 0.064(2) -0.0096(15) -0.0009(17) 0.0012(14) C9 0.059(2) 0.0275(15) 0.051(2) 0.0091(14) -0.0140(16) -0.0171(15) C10 0.0473(18) 0.0427(17) 0.0323(16) 0.0101(13) -0.0007(13) -0.0180(14) C11 0.0365(16) 0.0325(15) 0.0282(14) 0.0023(11) 0.0034(12) -0.0063(12) C12 0.0337(15) 0.0293(14) 0.0219(13) 0.0002(10) 0.0002(11) -0.0053(11) C13 0.0474(19) 0.0448(18) 0.0379(17) -0.0107(14) -0.0112(14) 0.0101(15) C14 0.068(2) 0.0407(18) 0.044(2) 0.0022(15) -0.0272(18) 0.0030(17) C15 0.078(3) 0.0467(19) 0.0230(15) 0.0066(14) -0.0083(16) -0.0196(18) C16 0.061(2) 0.053(2) 0.0295(16) -0.0057(14) 0.0135(15) -0.0124(17) C17 0.0380(17) 0.0408(16) 0.0288(15) 0.0000(12) 0.0048(12) -0.0033(13) C18 0.053(2) 0.053(2) 0.0335(17) 0.0173(14) -0.0105(14) -0.0140(16) C19 0.0378(17) 0.0405(17) 0.0397(17) 0.0044(13) -0.0120(13) -0.0056(13) C20 0.052(2) 0.078(3) 0.0415(19) -0.0071(18) -0.0052(16) 0.0353(19) C21 0.059(2) 0.053(2) 0.051(2) 0.0263(17) -0.0125(17) -0.0166(17) C22 0.0404(18) 0.065(2) 0.0407(18) -0.0044(16) 0.0118(14) -0.0149(16) C23 0.0305(15) 0.0325(15) 0.0444(17) 0.0044(13) 0.0022(13) -0.0076(12) C24 0.0158(12) 0.0213(12) 0.0248(13) -0.0043(10) -0.0012(10) -0.0004(9) C25 0.0187(12) 0.0253(13) 0.0235(13) -0.0018(10) -0.0026(10) 0.0000(10) C26 0.0234(13) 0.0318(14) 0.0231(13) -0.0060(10) -0.0002(10) 0.0001(11) C27 0.0217(13) 0.0245(13) 0.0305(14) -0.0101(11) -0.0012(11) 0.0007(10) C28 0.0220(13) 0.0189(12) 0.0320(14) -0.0036(10) -0.0025(11) -0.0005(10) C29 0.0175(12) 0.0209(12) 0.0267(13) -0.0039(10) -0.0025(10) -0.0030(9) C30 0.0280(14) 0.0358(15) 0.0274(14) 0.0054(11) 0.0029(11) 0.0075(12) C31 0.059(2) 0.057(2) 0.0304(16) 0.0125(15) 0.0112(15) 0.0209(17) C32 0.0346(16) 0.0309(15) 0.0425(17) 0.0096(12) 0.0077(13) 0.0037(12) C33 0.0332(16) 0.0512(19) 0.0345(16) 0.0086(14) -0.0060(13) 0.0094(14) C34 0.0351(16) 0.0321(15) 0.0403(16) -0.0117(12) 0.0052(13) 0.0064(12) C35 0.0244(13) 0.0256(13) 0.0272(13) 0.0008(10) 0.0003(11) 0.0019(10) C36 0.0413(17) 0.0395(16) 0.0292(15) -0.0069(12) 0.0006(13) 0.0046(13) C37 0.0289(15) 0.0355(15) 0.0444(17) 0.0102(13) 0.0065(13) 0.0004(12) C38 0.0363(16) 0.0347(15) 0.0336(15) 0.0065(12) 0.0022(12) 0.0074(12) C39 0.0210(13) 0.0379(15) 0.0368(16) 0.0024(12) 0.0022(11) -0.0011(11) C40 0.0207(13) 0.0358(15) 0.0333(15) 0.0012(12) -0.0052(11) -0.0069(11) C41 0.0330(16) 0.0390(16) 0.0378(16) -0.0077(13) 0.0083(13) 0.0022(13) C42 0.0379(17) 0.0359(16) 0.0388(16) -0.0160(13) -0.0019(13) -0.0069(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 Sm1 O1 2.1886(16) . ? Sm1 N4 2.399(2) . ? Sm1 N2 2.415(2) . ? Sm1 O2 2.5382(18) . ? Sm1 N1 2.541(2) . ? Sm1 O3 2.5813(17) . ? Sm1 N3 2.652(2) . ? Sm1 C1 2.884(2) . ? Sm1 C2 2.946(2) . ? Si1 N1 1.730(2) . ? Si1 C18 1.859(3) . ? Si1 C19 1.861(3) . ? Si1 C20 1.869(3) . ? Si2 N3 1.733(2) . ? Si2 C21 1.864(3) . ? Si2 C23 1.865(3) . ? Si2 C22 1.878(3) . ? O1 C24 1.346(3) . ? O2 C39 1.424(3) . ? O2 C41 1.427(3) . ? O3 C40 1.434(3) . ? O3 C42 1.435(3) . ? N1 C1 1.336(3) . ? N2 C1 1.311(3) . ? N2 C3 1.457(3) . ? N3 C2 1.331(3) . ? N4 C2 1.312(3) . ? N4 C5 1.459(4) . ? C1 C6 1.505(3) . ? C2 C12 1.514(4) . ? C3 C4 1.490(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.482(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.382(4) . ? C6 C11 1.386(4) . ? C7 C8 1.390(4) . ? C7 H7 0.9500 . ? C8 C9 1.368(5) . ? C8 H8 0.9500 . ? C9 C10 1.370(5) . ? C9 H9 0.9500 . ? C10 C11 1.384(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.381(4) . ? C12 C17 1.384(4) . ? C13 C14 1.384(4) . ? C13 H13 0.9500 . ? C14 C15 1.368(5) . ? C14 H14 0.9500 . ? C15 C16 1.362(5) . ? C15 H15 0.9500 . ? C16 C17 1.393(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? 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 1.423(3) . ? C24 C25 1.431(3) . ? C25 C26 1.395(3) . ? C25 C30 1.541(3) . ? C26 C27 1.380(4) . ? C26 H26 0.9500 . ? C27 C28 1.383(4) . ? C27 C34 1.508(3) . ? C28 C29 1.394(3) . ? C28 H28 0.9500 . ? C29 C35 1.536(4) . ? C30 C33 1.529(4) . ? C30 C32 1.535(4) . ? C30 C31 1.539(4) . ? 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 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.529(4) . ? C35 C37 1.536(4) . ? C35 C38 1.537(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.503(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 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 O1 Sm1 N4 110.62(8) . . ? O1 Sm1 N2 94.07(7) . . ? N4 Sm1 N2 70.65(8) . . ? O1 Sm1 O2 143.37(6) . . ? N4 Sm1 O2 102.26(7) . . ? N2 Sm1 O2 112.10(7) . . ? O1 Sm1 N1 109.19(6) . . ? N4 Sm1 N1 112.38(8) . . ? N2 Sm1 N1 54.13(7) . . ? O2 Sm1 N1 70.81(6) . . ? O1 Sm1 O3 82.84(6) . . ? N4 Sm1 O3 136.91(7) . . ? N2 Sm1 O3 151.47(7) . . ? O2 Sm1 O3 61.81(6) . . ? N1 Sm1 O3 100.03(6) . . ? O1 Sm1 N3 109.70(6) . . ? N4 Sm1 N3 52.68(7) . . ? N2 Sm1 N3 122.99(7) . . ? O2 Sm1 N3 77.79(6) . . ? N1 Sm1 N3 141.11(7) . . ? O3 Sm1 N3 84.25(6) . . ? O1 Sm1 C1 105.67(6) . . ? N4 Sm1 C1 89.45(8) . . ? N2 Sm1 C1 26.82(7) . . ? O2 Sm1 C1 89.97(6) . . ? N1 Sm1 C1 27.60(7) . . ? O3 Sm1 C1 127.39(6) . . ? N3 Sm1 C1 135.10(7) . . ? O1 Sm1 C2 111.15(7) . . ? N4 Sm1 C2 25.91(7) . . ? N2 Sm1 C2 96.53(7) . . ? O2 Sm1 C2 91.55(7) . . ? N1 Sm1 C2 131.20(7) . . ? O3 Sm1 C2 111.09(7) . . ? N3 Sm1 C2 26.85(7) . . ? C1 Sm1 C2 113.23(7) . . ? N1 Si1 C18 114.49(13) . . ? N1 Si1 C19 107.85(12) . . ? C18 Si1 C19 106.83(15) . . ? N1 Si1 C20 113.74(13) . . ? C18 Si1 C20 107.03(18) . . ? C19 Si1 C20 106.40(17) . . ? N3 Si2 C21 114.91(14) . . ? N3 Si2 C23 109.54(12) . . ? C21 Si2 C23 105.14(15) . . ? N3 Si2 C22 112.70(14) . . ? C21 Si2 C22 106.65(17) . . ? C23 Si2 C22 107.39(15) . . ? C24 O1 Sm1 178.87(16) . . ? C39 O2 C41 112.8(2) . . ? C39 O2 Sm1 118.41(15) . . ? C41 O2 Sm1 108.31(15) . . ? C40 O3 C42 110.5(2) . . ? C40 O3 Sm1 121.76(15) . . ? C42 O3 Sm1 126.21(16) . . ? C1 N1 Si1 127.50(17) . . ? C1 N1 Sm1 90.63(14) . . ? Si1 N1 Sm1 141.30(11) . . ? C1 N2 C3 121.4(2) . . ? C1 N2 Sm1 96.97(15) . . ? C3 N2 Sm1 138.24(17) . . ? C2 N3 Si2 125.00(18) . . ? C2 N3 Sm1 89.00(15) . . ? Si2 N3 Sm1 145.85(11) . . ? C2 N4 C5 122.2(2) . . ? C2 N4 Sm1 101.03(16) . . ? C5 N4 Sm1 136.49(18) . . ? N2 C1 N1 117.0(2) . . ? N2 C1 C6 120.0(2) . . ? N1 C1 C6 122.9(2) . . ? N2 C1 Sm1 56.21(13) . . ? N1 C1 Sm1 61.76(12) . . ? C6 C1 Sm1 169.90(17) . . ? N4 C2 N3 117.0(2) . . ? N4 C2 C12 120.0(2) . . ? N3 C2 C12 123.0(2) . . ? N4 C2 Sm1 53.06(13) . . ? N3 C2 Sm1 64.16(13) . . ? C12 C2 Sm1 171.33(18) . . ? N2 C3 C4 111.9(2) . . ? N2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 115.5(3) . . ? C5 C4 H4A 108.4 . . ? C3 C4 H4A 108.4 . . ? C5 C4 H4B 108.4 . . ? C3 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? N4 C5 C4 111.5(2) . . ? N4 C5 H5A 109.3 . . ? C4 C5 H5A 109.3 . . ? N4 C5 H5B 109.3 . . ? C4 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C7 C6 C11 119.2(2) . . ? C7 C6 C1 121.5(2) . . ? C11 C6 C1 119.3(2) . . ? C6 C7 C8 119.6(3) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 120.8(3) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 119.8(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 120.2(3) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C6 120.4(3) . . ? C10 C11 H11 119.8 . . ? C6 C11 H11 119.8 . . ? C13 C12 C17 118.6(3) . . ? C13 C12 C2 121.0(3) . . ? C17 C12 C2 120.3(2) . . ? C12 C13 C14 120.9(3) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 120.0(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.6(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C12 C17 C16 120.0(3) . . ? C12 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O1 C24 C29 120.5(2) . . ? O1 C24 C25 120.5(2) . . ? C29 C24 C25 119.0(2) . . ? C26 C25 C24 118.0(2) . . ? C26 C25 C30 119.4(2) . . ? C24 C25 C30 122.7(2) . . ? C27 C26 C25 123.7(2) . . ? C27 C26 H26 118.1 . . ? C25 C26 H26 118.1 . . ? C26 C27 C28 117.4(2) . . ? C26 C27 C34 121.7(2) . . ? C28 C27 C34 121.0(2) . . ? C27 C28 C29 123.0(2) . . ? C27 C28 H28 118.5 . . ? C29 C28 H28 118.5 . . ? C28 C29 C24 118.9(2) . . ? C28 C29 C35 119.0(2) . . ? C24 C29 C35 122.1(2) . . ? C33 C30 C32 110.1(2) . . ? C33 C30 C31 106.7(2) . . ? C32 C30 C31 106.5(2) . . ? C33 C30 C25 110.6(2) . . ? C32 C30 C25 110.5(2) . . ? C31 C30 C25 112.4(2) . . ? 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 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C27 C34 H34A 109.5 . . ? C27 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C27 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C29 110.7(2) . . ? C36 C35 C37 110.5(2) . . ? C29 C35 C37 109.8(2) . . ? C36 C35 C38 106.8(2) . . ? C29 C35 C38 112.9(2) . . ? C37 C35 C38 106.0(2) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O2 C39 C40 107.9(2) . . ? O2 C39 H39A 110.1 . . ? C40 C39 H39A 110.1 . . ? O2 C39 H39B 110.1 . . ? C40 C39 H39B 110.1 . . ? H39A C39 H39B 108.4 . . ? O3 C40 C39 109.0(2) . . ? O3 C40 H40A 109.9 . . ? C39 C40 H40A 109.9 . . ? O3 C40 H40B 109.9 . . ? C39 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? O2 C41 H41A 109.5 . . ? O2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O3 C42 H42A 109.5 . . ? O3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 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 N4 Sm1 O1 C24 -18(8) . . . . ? N2 Sm1 O1 C24 -89(8) . . . . ? O2 Sm1 O1 C24 134(8) . . . . ? N1 Sm1 O1 C24 -142(8) . . . . ? O3 Sm1 O1 C24 120(8) . . . . ? N3 Sm1 O1 C24 38(8) . . . . ? C1 Sm1 O1 C24 -114(8) . . . . ? C2 Sm1 O1 C24 10(8) . . . . ? O1 Sm1 O2 C39 -45.1(2) . . . . ? N4 Sm1 O2 C39 108.64(18) . . . . ? N2 Sm1 O2 C39 -177.48(17) . . . . ? N1 Sm1 O2 C39 -141.66(18) . . . . ? O3 Sm1 O2 C39 -28.36(16) . . . . ? N3 Sm1 O2 C39 61.63(17) . . . . ? C1 Sm1 O2 C39 -161.92(18) . . . . ? C2 Sm1 O2 C39 84.84(18) . . . . ? O1 Sm1 O2 C41 -175.04(15) . . . . ? N4 Sm1 O2 C41 -21.35(17) . . . . ? N2 Sm1 O2 C41 52.53(18) . . . . ? N1 Sm1 O2 C41 88.35(17) . . . . ? O3 Sm1 O2 C41 -158.35(18) . . . . ? N3 Sm1 O2 C41 -68.36(16) . . . . ? C1 Sm1 O2 C41 68.09(17) . . . . ? C2 Sm1 O2 C41 -45.15(17) . . . . ? O1 Sm1 O3 C40 170.38(18) . . . . ? N4 Sm1 O3 C40 -77.0(2) . . . . ? N2 Sm1 O3 C40 85.0(2) . . . . ? O2 Sm1 O3 C40 0.33(17) . . . . ? N1 Sm1 O3 C40 62.07(18) . . . . ? N3 Sm1 O3 C40 -78.88(18) . . . . ? C1 Sm1 O3 C40 66.11(19) . . . . ? C2 Sm1 O3 C40 -79.66(18) . . . . ? O1 Sm1 O3 C42 6.1(2) . . . . ? N4 Sm1 O3 C42 118.7(2) . . . . ? N2 Sm1 O3 C42 -79.3(2) . . . . ? O2 Sm1 O3 C42 -164.0(2) . . . . ? N1 Sm1 O3 C42 -102.3(2) . . . . ? N3 Sm1 O3 C42 116.8(2) . . . . ? C1 Sm1 O3 C42 -98.2(2) . . . . ? C2 Sm1 O3 C42 116.0(2) . . . . ? C18 Si1 N1 C1 -38.2(3) . . . . ? C19 Si1 N1 C1 -156.9(2) . . . . ? C20 Si1 N1 C1 85.3(3) . . . . ? C18 Si1 N1 Sm1 153.29(18) . . . . ? C19 Si1 N1 Sm1 34.5(2) . . . . ? C20 Si1 N1 Sm1 -83.2(2) . . . . ? O1 Sm1 N1 C1 87.22(14) . . . . ? N4 Sm1 N1 C1 -35.91(16) . . . . ? N2 Sm1 N1 C1 6.36(13) . . . . ? O2 Sm1 N1 C1 -131.64(15) . . . . ? O3 Sm1 N1 C1 173.07(14) . . . . ? N3 Sm1 N1 C1 -93.65(16) . . . . ? C2 Sm1 N1 C1 -57.11(17) . . . . ? O1 Sm1 N1 Si1 -101.87(17) . . . . ? N4 Sm1 N1 Si1 135.00(17) . . . . ? N2 Sm1 N1 Si1 177.3(2) . . . . ? O2 Sm1 N1 Si1 39.27(16) . . . . ? O3 Sm1 N1 Si1 -16.02(18) . . . . ? N3 Sm1 N1 Si1 77.3(2) . . . . ? C1 Sm1 N1 Si1 170.9(3) . . . . ? C2 Sm1 N1 Si1 113.80(17) . . . . ? O1 Sm1 N2 C1 -117.34(16) . . . . ? N4 Sm1 N2 C1 132.22(18) . . . . ? O2 Sm1 N2 C1 36.46(17) . . . . ? N1 Sm1 N2 C1 -6.54(14) . . . . ? O3 Sm1 N2 C1 -34.8(2) . . . . ? N3 Sm1 N2 C1 125.98(15) . . . . ? C2 Sm1 N2 C1 130.81(16) . . . . ? O1 Sm1 N2 C3 85.1(3) . . . . ? N4 Sm1 N2 C3 -25.3(3) . . . . ? O2 Sm1 N2 C3 -121.1(3) . . . . ? N1 Sm1 N2 C3 -164.1(3) . . . . ? O3 Sm1 N2 C3 167.6(2) . . . . ? N3 Sm1 N2 C3 -31.6(3) . . . . ? C1 Sm1 N2 C3 -157.6(4) . . . . ? C2 Sm1 N2 C3 -26.7(3) . . . . ? C21 Si2 N3 C2 45.4(3) . . . . ? C23 Si2 N3 C2 163.5(2) . . . . ? C22 Si2 N3 C2 -77.1(3) . . . . ? C21 Si2 N3 Sm1 -128.4(2) . . . . ? C23 Si2 N3 Sm1 -10.3(2) . . . . ? C22 Si2 N3 Sm1 109.2(2) . . . . ? O1 Sm1 N3 C2 -98.12(15) . . . . ? N4 Sm1 N3 C2 3.27(15) . . . . ? N2 Sm1 N3 C2 10.68(18) . . . . ? O2 Sm1 N3 C2 119.25(15) . . . . ? N1 Sm1 N3 C2 82.76(18) . . . . ? O3 Sm1 N3 C2 -178.39(15) . . . . ? C1 Sm1 N3 C2 41.83(19) . . . . ? O1 Sm1 N3 Si2 76.8(2) . . . . ? N4 Sm1 N3 Si2 178.2(2) . . . . ? N2 Sm1 N3 Si2 -174.42(18) . . . . ? O2 Sm1 N3 Si2 -65.8(2) . . . . ? N1 Sm1 N3 Si2 -102.3(2) . . . . ? O3 Sm1 N3 Si2 -3.5(2) . . . . ? C1 Sm1 N3 Si2 -143.27(18) . . . . ? C2 Sm1 N3 Si2 174.9(3) . . . . ? O1 Sm1 N4 C2 96.18(18) . . . . ? N2 Sm1 N4 C2 -176.8(2) . . . . ? O2 Sm1 N4 C2 -67.42(19) . . . . ? N1 Sm1 N4 C2 -141.50(17) . . . . ? O3 Sm1 N4 C2 -5.8(2) . . . . ? N3 Sm1 N4 C2 -3.38(16) . . . . ? C1 Sm1 N4 C2 -157.27(19) . . . . ? O1 Sm1 N4 C5 -77.0(3) . . . . ? N2 Sm1 N4 C5 10.0(3) . . . . ? O2 Sm1 N4 C5 119.4(3) . . . . ? N1 Sm1 N4 C5 45.3(3) . . . . ? O3 Sm1 N4 C5 -179.0(3) . . . . ? N3 Sm1 N4 C5 -176.6(4) . . . . ? C1 Sm1 N4 C5 29.6(3) . . . . ? C2 Sm1 N4 C5 -173.2(5) . . . . ? C3 N2 C1 N1 174.0(2) . . . . ? Sm1 N2 C1 N1 11.4(2) . . . . ? C3 N2 C1 C6 -6.3(4) . . . . ? Sm1 N2 C1 C6 -168.95(19) . . . . ? C3 N2 C1 Sm1 162.7(3) . . . . ? Si1 N1 C1 N2 176.45(18) . . . . ? Sm1 N1 C1 N2 -10.7(2) . . . . ? Si1 N1 C1 C6 -3.2(4) . . . . ? Sm1 N1 C1 C6 169.6(2) . . . . ? Si1 N1 C1 Sm1 -172.9(2) . . . . ? O1 Sm1 C1 N2 66.96(17) . . . . ? N4 Sm1 C1 N2 -44.33(17) . . . . ? O2 Sm1 C1 N2 -146.59(16) . . . . ? N1 Sm1 C1 N2 168.5(2) . . . . ? O3 Sm1 C1 N2 159.92(14) . . . . ? N3 Sm1 C1 N2 -74.05(18) . . . . ? C2 Sm1 C1 N2 -54.92(17) . . . . ? O1 Sm1 C1 N1 -101.56(14) . . . . ? N4 Sm1 C1 N1 147.15(15) . . . . ? N2 Sm1 C1 N1 -168.5(2) . . . . ? O2 Sm1 C1 N1 44.89(14) . . . . ? O3 Sm1 C1 N1 -8.60(17) . . . . ? N3 Sm1 C1 N1 117.43(14) . . . . ? C2 Sm1 C1 N1 136.57(14) . . . . ? O1 Sm1 C1 C6 138.1(10) . . . . ? N4 Sm1 C1 C6 26.8(10) . . . . ? N2 Sm1 C1 C6 71.1(10) . . . . ? O2 Sm1 C1 C6 -75.5(10) . . . . ? N1 Sm1 C1 C6 -120.4(11) . . . . ? O3 Sm1 C1 C6 -129.0(10) . . . . ? N3 Sm1 C1 C6 -2.9(11) . . . . ? C2 Sm1 C1 C6 16.2(10) . . . . ? C5 N4 C2 N3 -179.5(3) . . . . ? Sm1 N4 C2 N3 6.0(3) . . . . ? C5 N4 C2 C12 0.7(4) . . . . ? Sm1 N4 C2 C12 -173.7(2) . . . . ? C5 N4 C2 Sm1 174.5(4) . . . . ? Si2 N3 C2 N4 178.2(2) . . . . ? Sm1 N3 C2 N4 -5.3(2) . . . . ? Si2 N3 C2 C12 -2.1(4) . . . . ? Sm1 N3 C2 C12 174.4(2) . . . . ? Si2 N3 C2 Sm1 -176.5(2) . . . . ? O1 Sm1 C2 N4 -93.89(19) . . . . ? N2 Sm1 C2 N4 3.0(2) . . . . ? O2 Sm1 C2 N4 115.50(19) . . . . ? N1 Sm1 C2 N4 49.9(2) . . . . ? O3 Sm1 C2 N4 175.76(18) . . . . ? N3 Sm1 C2 N4 174.0(3) . . . . ? C1 Sm1 C2 N4 24.9(2) . . . . ? O1 Sm1 C2 N3 92.06(15) . . . . ? N4 Sm1 C2 N3 -174.0(3) . . . . ? N2 Sm1 C2 N3 -171.00(15) . . . . ? O2 Sm1 C2 N3 -58.55(15) . . . . ? N1 Sm1 C2 N3 -124.13(15) . . . . ? O3 Sm1 C2 N3 1.72(16) . . . . ? C1 Sm1 C2 N3 -149.18(14) . . . . ? O1 Sm1 C2 C12 -55.2(12) . . . . ? N4 Sm1 C2 C12 38.7(12) . . . . ? N2 Sm1 C2 C12 41.8(12) . . . . ? O2 Sm1 C2 C12 154.2(12) . . . . ? N1 Sm1 C2 C12 88.6(12) . . . . ? O3 Sm1 C2 C12 -145.5(12) . . . . ? N3 Sm1 C2 C12 -147.2(13) . . . . ? C1 Sm1 C2 C12 63.6(12) . . . . ? C1 N2 C3 C4 -154.1(3) . . . . ? Sm1 N2 C3 C4 -0.5(4) . . . . ? N2 C3 C4 C5 56.6(4) . . . . ? C2 N4 C5 C4 -144.4(3) . . . . ? Sm1 N4 C5 C4 27.7(5) . . . . ? C3 C4 C5 N4 -69.3(4) . . . . ? N2 C1 C6 C7 105.2(3) . . . . ? N1 C1 C6 C7 -75.1(3) . . . . ? Sm1 C1 C6 C7 40.0(11) . . . . ? N2 C1 C6 C11 -73.9(3) . . . . ? N1 C1 C6 C11 105.8(3) . . . . ? Sm1 C1 C6 C11 -139.1(9) . . . . ? C11 C6 C7 C8 -1.1(4) . . . . ? C1 C6 C7 C8 179.8(3) . . . . ? C6 C7 C8 C9 -0.3(5) . . . . ? C7 C8 C9 C10 1.1(5) . . . . ? C8 C9 C10 C11 -0.5(5) . . . . ? C9 C10 C11 C6 -0.8(4) . . . . ? C7 C6 C11 C10 1.6(4) . . . . ? C1 C6 C11 C10 -179.2(3) . . . . ? N4 C2 C12 C13 78.4(4) . . . . ? N3 C2 C12 C13 -101.4(3) . . . . ? Sm1 C2 C12 C13 43.1(13) . . . . ? N4 C2 C12 C17 -98.7(3) . . . . ? N3 C2 C12 C17 81.5(3) . . . . ? Sm1 C2 C12 C17 -134.0(11) . . . . ? C17 C12 C13 C14 -2.1(5) . . . . ? C2 C12 C13 C14 -179.3(3) . . . . ? C12 C13 C14 C15 1.3(5) . . . . ? C13 C14 C15 C16 0.3(5) . . . . ? C14 C15 C16 C17 -1.0(5) . . . . ? C13 C12 C17 C16 1.4(4) . . . . ? C2 C12 C17 C16 178.6(3) . . . . ? C15 C16 C17 C12 0.1(5) . . . . ? Sm1 O1 C24 C29 -31(8) . . . . ? Sm1 O1 C24 C25 150(8) . . . . ? O1 C24 C25 C26 178.3(2) . . . . ? C29 C24 C25 C26 -1.1(3) . . . . ? O1 C24 C25 C30 -2.0(4) . . . . ? C29 C24 C25 C30 178.6(2) . . . . ? C24 C25 C26 C27 1.2(4) . . . . ? C30 C25 C26 C27 -178.5(2) . . . . ? C25 C26 C27 C28 0.1(4) . . . . ? C25 C26 C27 C34 -179.5(2) . . . . ? C26 C27 C28 C29 -1.5(4) . . . . ? C34 C27 C28 C29 178.0(2) . . . . ? C27 C28 C29 C24 1.5(4) . . . . ? C27 C28 C29 C35 -177.2(2) . . . . ? O1 C24 C29 C28 -179.6(2) . . . . ? C25 C24 C29 C28 -0.2(3) . . . . ? O1 C24 C29 C35 -0.9(3) . . . . ? C25 C24 C29 C35 178.5(2) . . . . ? C26 C25 C30 C33 -118.7(3) . . . . ? C24 C25 C30 C33 61.6(3) . . . . ? C26 C25 C30 C32 119.1(3) . . . . ? C24 C25 C30 C32 -60.5(3) . . . . ? C26 C25 C30 C31 0.3(4) . . . . ? C24 C25 C30 C31 -179.4(3) . . . . ? C28 C29 C35 C36 -120.9(2) . . . . ? C24 C29 C35 C36 60.5(3) . . . . ? C28 C29 C35 C37 116.8(2) . . . . ? C24 C29 C35 C37 -61.8(3) . . . . ? C28 C29 C35 C38 -1.2(3) . . . . ? C24 C29 C35 C38 -179.8(2) . . . . ? C41 O2 C39 C40 179.3(2) . . . . ? Sm1 O2 C39 C40 51.4(2) . . . . ? C42 O3 C40 C39 -169.3(2) . . . . ? Sm1 O3 C40 C39 24.2(3) . . . . ? O2 C39 C40 O3 -46.0(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.404 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.069 data_complex6 _database_code_depnum_ccdc_archive 'CCDC 915748' #TrackingRef '915748.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H67 N4 O3 Si2 Yb' _chemical_formula_sum 'C42 H67 N4 O3 Si2 Yb' _chemical_formula_weight 905.22 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.7177(9) _cell_length_b 9.1356(3) _cell_length_c 21.8886(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.3490(10) _cell_angle_gamma 90.00 _cell_volume 4541.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13795 _cell_measurement_theta_min 3.0? _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1876 _exptl_absorpt_coefficient_mu 2.151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.362 _exptl_absorpt_correction_T_max 0.525 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32573 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_unetI/netI 0.0612 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10281 _reflns_number_gt 9220 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Their C3-H3A,C3-H3B,C5-H5A, C5-H5B,C3-C4,C3-C4',C14-C15 and C15-C16 distances were constrained. ; _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^)+(0.0343P)^2^+4.3310P] 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 10281 _refine_ls_number_parameters 470 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0858 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.082 _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 Yb1 Yb 0.253307(6) 0.235876(14) 0.351563(6) 0.03046(6) Uani 1 1 d . . . Si1 Si 0.09396(4) 0.05009(11) 0.40013(5) 0.0430(2) Uani 1 1 d . . . Si2 Si 0.40887(5) 0.06129(14) 0.30017(6) 0.0570(3) Uani 1 1 d . . . O1 O 0.22985(10) 0.3894(2) 0.28321(11) 0.0369(5) Uani 1 1 d . . . O2 O 0.27327(12) -0.0060(3) 0.39640(13) 0.0533(7) Uani 1 1 d . . . O3 O 0.22933(11) 0.0392(3) 0.28406(12) 0.0430(6) Uani 1 1 d . . . N1 N 0.15640(12) 0.1599(3) 0.40249(13) 0.0363(6) Uani 1 1 d . . . N2 N 0.22330(15) 0.3132(4) 0.44398(14) 0.0578(10) Uani 1 1 d . A . N3 N 0.35977(13) 0.1819(4) 0.33319(15) 0.0449(7) Uani 1 1 d . . . N4 N 0.33056(13) 0.3640(4) 0.39426(16) 0.0519(8) Uani 1 1 d . A . C1 C 0.17169(17) 0.2472(4) 0.44898(16) 0.0389(8) Uani 1 1 d . . . C2 C 0.37324(16) 0.2801(5) 0.37604(19) 0.0474(9) Uani 1 1 d . . . C3 C 0.2412(2) 0.4211(8) 0.4903(2) 0.0863(19) Uani 1 1 d D . . H3A H 0.272(2) 0.362(6) 0.511(3) 0.104 Uiso 1 1 d D . . H3B H 0.2160(19) 0.435(6) 0.5254(16) 0.104 Uiso 1 1 d D . . C4 C 0.2830(4) 0.5258(9) 0.4675(4) 0.0550(15) Uani 0.50 1 d PD A 1 H4A H 0.2928 0.5932 0.5010 0.066 Uiso 0.50 1 calc PR A 1 H4B H 0.2625 0.5834 0.4357 0.066 Uiso 0.50 1 calc PR A 1 C4' C 0.3053(4) 0.4419(10) 0.4969(4) 0.0550(15) Uani 0.50 1 d PD A 2 H4'A H 0.3123 0.5209 0.5264 0.066 Uiso 0.50 1 calc PR A 2 H4'B H 0.3220 0.3524 0.5149 0.066 Uiso 0.50 1 calc PR A 2 C5 C 0.3385(2) 0.4761(6) 0.4421(2) 0.0672(14) Uani 1 1 d D . . H5A H 0.3746(13) 0.456(5) 0.4663(19) 0.081 Uiso 1 1 d D . . H5B H 0.355(2) 0.564(3) 0.422(2) 0.081 Uiso 1 1 d D . . C6 C 0.13548(17) 0.2635(4) 0.50523(17) 0.0420(8) Uani 1 1 d . . . C7 C 0.09413(18) 0.3752(5) 0.50998(18) 0.0522(10) Uani 1 1 d . . . H7 H 0.0892 0.4430 0.4780 0.063 Uiso 1 1 calc R . . C8 C 0.06051(19) 0.3871(5) 0.5611(2) 0.0601(11) Uani 1 1 d . . . H8 H 0.0322 0.4618 0.5634 0.072 Uiso 1 1 calc R . . C9 C 0.0679(2) 0.2908(5) 0.6087(2) 0.0659(13) Uani 1 1 d . . . H9 H 0.0445 0.2987 0.6433 0.079 Uiso 1 1 calc R . . C10 C 0.1100(3) 0.1822(6) 0.6054(2) 0.0739(14) Uani 1 1 d . . . H10 H 0.1159 0.1173 0.6383 0.089 Uiso 1 1 calc R . . C11 C 0.1433(2) 0.1692(5) 0.55404(18) 0.0578(11) Uani 1 1 d . . . H11 H 0.1719 0.0951 0.5521 0.069 Uiso 1 1 calc R . . C12 C 0.4341(2) 0.2960(8) 0.4045(3) 0.0935(8) Uani 1 1 d . . . C13 C 0.4522(2) 0.1990(8) 0.4497(3) 0.0935(8) Uani 1 1 d . . . H13 H 0.4268 0.1234 0.4615 0.112 Uiso 1 1 calc R . . C14 C 0.5073(2) 0.2116(7) 0.4781(3) 0.0935(8) Uani 1 1 d D . . H14 H 0.5194 0.1467 0.5092 0.112 Uiso 1 1 calc R . . C15 C 0.5426(2) 0.3199(7) 0.4593(3) 0.0935(8) Uani 1 1 d D . . H15 H 0.5805 0.3261 0.4772 0.112 Uiso 1 1 calc R . . C16 C 0.5273(2) 0.4214(7) 0.4162(3) 0.0935(8) Uani 1 1 d D . . H16 H 0.5532 0.4967 0.4052 0.112 Uiso 1 1 calc R . . C17 C 0.4706(2) 0.4078(7) 0.3888(3) 0.0935(8) Uani 1 1 d . . . H17 H 0.4579 0.4767 0.3595 0.112 Uiso 1 1 calc R . . C18 C 0.0975(2) -0.1077(5) 0.4551(2) 0.0722(14) Uani 1 1 d . . . H18A H 0.1355 -0.1555 0.4526 0.108 Uiso 1 1 calc R . . H18B H 0.0665 -0.1772 0.4448 0.108 Uiso 1 1 calc R . . H18C H 0.0922 -0.0719 0.4963 0.108 Uiso 1 1 calc R . . C19 C 0.08604(16) -0.0317(4) 0.32222(18) 0.0460(9) Uani 1 1 d . . . H19A H 0.0837 0.0458 0.2920 0.069 Uiso 1 1 calc R . . H19B H 0.0504 -0.0903 0.3198 0.069 Uiso 1 1 calc R . . H19C H 0.1198 -0.0933 0.3144 0.069 Uiso 1 1 calc R . . C20 C 0.02254(18) 0.1460(6) 0.4146(2) 0.0685(13) Uani 1 1 d . . . H20A H 0.0184 0.1603 0.4582 0.103 Uiso 1 1 calc R . . H20B H -0.0099 0.0870 0.3989 0.103 Uiso 1 1 calc R . . H20C H 0.0222 0.2403 0.3943 0.103 Uiso 1 1 calc R . . C21 C 0.4226(3) -0.1022(7) 0.3503(3) 0.114(3) Uani 1 1 d . . . H21A H 0.4491 -0.0755 0.3838 0.171 Uiso 1 1 calc R . . H21B H 0.4400 -0.1798 0.3265 0.171 Uiso 1 1 calc R . . H21C H 0.3856 -0.1359 0.3665 0.171 Uiso 1 1 calc R . . C22 C 0.4804(2) 0.1477(8) 0.2797(4) 0.118(3) Uani 1 1 d . . . H22A H 0.4730 0.2439 0.2624 0.177 Uiso 1 1 calc R . . H22B H 0.4999 0.0870 0.2500 0.177 Uiso 1 1 calc R . . H22C H 0.5053 0.1569 0.3161 0.177 Uiso 1 1 calc R . . C23 C 0.3784(2) -0.0128(6) 0.2269(2) 0.0709(13) Uani 1 1 d . . . H23A H 0.3383 -0.0458 0.2327 0.106 Uiso 1 1 calc R . . H23B H 0.4023 -0.0945 0.2139 0.106 Uiso 1 1 calc R . . H23C H 0.3786 0.0632 0.1960 0.106 Uiso 1 1 calc R . . C24 C 0.21351(15) 0.4905(4) 0.24125(16) 0.0367(7) Uani 1 1 d . . . C25 C 0.25425(17) 0.5423(4) 0.19691(17) 0.0441(8) Uani 1 1 d . . . C26 C 0.2340(2) 0.6432(4) 0.15342(17) 0.0532(10) Uani 1 1 d . . . H26 H 0.2605 0.6757 0.1240 0.064 Uiso 1 1 calc R . . C27 C 0.1775(2) 0.6979(4) 0.15116(18) 0.0532(10) Uani 1 1 d . . . C28 C 0.13969(18) 0.6506(4) 0.19456(18) 0.0477(9) Uani 1 1 d . . . H28 H 0.1013 0.6890 0.1941 0.057 Uiso 1 1 calc R . . C29 C 0.15508(16) 0.5479(4) 0.23965(16) 0.0390(8) Uani 1 1 d . . . C30 C 0.31846(19) 0.4919(5) 0.1959(2) 0.0556(10) Uani 1 1 d . . . C31 C 0.3529(2) 0.5637(6) 0.1439(2) 0.0796(15) Uani 1 1 d . . . H31A H 0.3343 0.5389 0.1048 0.119 Uiso 1 1 calc R . . H31B H 0.3931 0.5282 0.1450 0.119 Uiso 1 1 calc R . . H31C H 0.3528 0.6691 0.1490 0.119 Uiso 1 1 calc R . . C32 C 0.3210(2) 0.3262(5) 0.1855(2) 0.0675(12) Uani 1 1 d . . . H32A H 0.3047 0.2760 0.2203 0.101 Uiso 1 1 calc R . . H32B H 0.3616 0.2963 0.1807 0.101 Uiso 1 1 calc R . . H32C H 0.2983 0.3014 0.1488 0.101 Uiso 1 1 calc R . . C33 C 0.35004(19) 0.5333(5) 0.2556(2) 0.0646(12) Uani 1 1 d . . . H33A H 0.3524 0.6390 0.2588 0.097 Uiso 1 1 calc R . . H33B H 0.3894 0.4923 0.2563 0.097 Uiso 1 1 calc R . . H33C H 0.3283 0.4949 0.2897 0.097 Uiso 1 1 calc R . . C34 C 0.1575(3) 0.8052(5) 0.1018(2) 0.0759(15) Uani 1 1 d . . . H34A H 0.1160 0.7907 0.0926 0.114 Uiso 1 1 calc R . . H34B H 0.1799 0.7888 0.0653 0.114 Uiso 1 1 calc R . . H34C H 0.1640 0.9045 0.1162 0.114 Uiso 1 1 calc R . . C35 C 0.10859(15) 0.4986(4) 0.28463(17) 0.0408(8) Uani 1 1 d . . . C36 C 0.04812(18) 0.5707(5) 0.2722(2) 0.0601(11) Uani 1 1 d . . . H36A H 0.0519 0.6761 0.2760 0.090 Uiso 1 1 calc R . . H36B H 0.0202 0.5352 0.3016 0.090 Uiso 1 1 calc R . . H36C H 0.0342 0.5462 0.2312 0.090 Uiso 1 1 calc R . . C37 C 0.12759(18) 0.5387(4) 0.35035(17) 0.0482(9) Uani 1 1 d . . . H37A H 0.1660 0.4968 0.3596 0.072 Uiso 1 1 calc R . . H37B H 0.0992 0.5002 0.3786 0.072 Uiso 1 1 calc R . . H37C H 0.1296 0.6443 0.3544 0.072 Uiso 1 1 calc R . . C38 C 0.09805(16) 0.3330(4) 0.27807(18) 0.0425(8) Uani 1 1 d . . . H38A H 0.0848 0.3113 0.2366 0.064 Uiso 1 1 calc R . . H38B H 0.0682 0.3024 0.3064 0.064 Uiso 1 1 calc R . . H38C H 0.1344 0.2810 0.2871 0.064 Uiso 1 1 calc R . . C39 C 0.2451(2) -0.1245(5) 0.3668(3) 0.0745(14) Uani 1 1 d . . . H39A H 0.2050 -0.1334 0.3818 0.089 Uiso 1 1 calc R . . H39B H 0.2662 -0.2149 0.3773 0.089 Uiso 1 1 calc R . . C40 C 0.2426(2) -0.1087(4) 0.3004(2) 0.0588(11) Uani 1 1 d . . . H40A H 0.2805 -0.1369 0.2835 0.071 Uiso 1 1 calc R . . H40B H 0.2122 -0.1738 0.2831 0.071 Uiso 1 1 calc R . . C41 C 0.2852(2) -0.0255(6) 0.4592(2) 0.0755(14) Uani 1 1 d . . . H41A H 0.2485 -0.0282 0.4809 0.113 Uiso 1 1 calc R . . H41B H 0.3092 0.0550 0.4744 0.113 Uiso 1 1 calc R . . H41C H 0.3062 -0.1169 0.4656 0.113 Uiso 1 1 calc R . . C42 C 0.20840(18) 0.0526(5) 0.22183(17) 0.0519(10) Uani 1 1 d . . . H42A H 0.2376 0.0133 0.1947 0.078 Uiso 1 1 calc R . . H42B H 0.2016 0.1549 0.2123 0.078 Uiso 1 1 calc R . . H42C H 0.1719 -0.0015 0.2165 0.078 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 0.03123(8) 0.03061(8) 0.02950(8) -0.00196(5) -0.00024(6) -0.00108(5) Si1 0.0415(5) 0.0435(6) 0.0443(6) 0.0002(4) 0.0069(5) -0.0080(4) Si2 0.0401(6) 0.0608(7) 0.0703(8) -0.0144(6) 0.0042(6) 0.0078(5) O1 0.0391(12) 0.0360(12) 0.0357(13) 0.0037(10) -0.0001(10) -0.0024(10) O2 0.0530(16) 0.0449(15) 0.0614(18) 0.0087(13) -0.0096(14) 0.0033(12) O3 0.0515(14) 0.0345(13) 0.0429(14) -0.0087(11) 0.0012(12) -0.0035(11) N1 0.0389(15) 0.0382(15) 0.0322(15) -0.0014(12) 0.0033(12) -0.0024(12) N2 0.058(2) 0.084(2) 0.0310(16) -0.0208(17) 0.0133(15) -0.0425(19) N3 0.0344(15) 0.0525(18) 0.0478(18) -0.0076(15) 0.0036(14) -0.0010(14) N4 0.0351(16) 0.068(2) 0.053(2) -0.0227(17) 0.0023(15) -0.0081(15) C1 0.0426(19) 0.044(2) 0.0304(17) 0.0004(14) 0.0066(15) 0.0042(14) C2 0.0344(18) 0.062(2) 0.046(2) -0.0034(19) 0.0021(17) -0.0054(17) C3 0.072(3) 0.131(5) 0.056(3) -0.051(3) 0.022(2) -0.044(3) C4 0.065(4) 0.049(4) 0.050(4) -0.016(3) -0.003(3) -0.010(3) C4' 0.065(4) 0.049(4) 0.050(4) -0.016(3) -0.003(3) -0.010(3) C5 0.053(2) 0.080(3) 0.068(3) -0.036(3) 0.006(2) -0.023(2) C6 0.044(2) 0.050(2) 0.0323(18) -0.0060(15) 0.0084(16) -0.0046(16) C7 0.056(2) 0.062(3) 0.038(2) 0.0008(18) 0.0050(18) 0.005(2) C8 0.058(2) 0.076(3) 0.047(2) -0.005(2) 0.012(2) 0.013(2) C9 0.082(3) 0.075(3) 0.042(2) -0.002(2) 0.031(2) 0.002(3) C10 0.113(4) 0.068(3) 0.042(2) 0.012(2) 0.028(3) 0.013(3) C11 0.080(3) 0.056(2) 0.038(2) 0.0034(18) 0.015(2) 0.014(2) C12 0.0606(13) 0.120(2) 0.0990(19) -0.0312(17) -0.0178(13) -0.0081(13) C13 0.0606(13) 0.120(2) 0.0990(19) -0.0312(17) -0.0178(13) -0.0081(13) C14 0.0606(13) 0.120(2) 0.0990(19) -0.0312(17) -0.0178(13) -0.0081(13) C15 0.0606(13) 0.120(2) 0.0990(19) -0.0312(17) -0.0178(13) -0.0081(13) C16 0.0606(13) 0.120(2) 0.0990(19) -0.0312(17) -0.0178(13) -0.0081(13) C17 0.0606(13) 0.120(2) 0.0990(19) -0.0312(17) -0.0178(13) -0.0081(13) C18 0.095(4) 0.062(3) 0.060(3) 0.014(2) 0.007(3) -0.023(3) C19 0.044(2) 0.039(2) 0.055(2) -0.0014(17) -0.0020(18) -0.0081(16) C20 0.041(2) 0.083(3) 0.082(3) -0.018(3) 0.016(2) -0.010(2) C21 0.165(7) 0.080(4) 0.098(5) -0.014(4) -0.020(5) 0.057(4) C22 0.051(3) 0.132(6) 0.172(7) -0.076(5) 0.041(4) -0.016(3) C23 0.060(3) 0.073(3) 0.080(3) -0.023(3) 0.017(3) 0.009(2) C24 0.0461(19) 0.0314(17) 0.0323(17) 0.0018(14) -0.0030(15) -0.0070(14) C25 0.057(2) 0.0390(19) 0.0365(19) 0.0007(15) 0.0040(17) -0.0116(16) C26 0.080(3) 0.044(2) 0.036(2) 0.0033(16) 0.004(2) -0.019(2) C27 0.081(3) 0.039(2) 0.039(2) 0.0085(17) -0.015(2) -0.012(2) C28 0.057(2) 0.0367(19) 0.048(2) 0.0024(17) -0.0165(19) -0.0047(17) C29 0.048(2) 0.0301(17) 0.0386(19) 0.0006(14) -0.0085(16) -0.0064(14) C30 0.057(2) 0.057(2) 0.053(2) 0.004(2) 0.015(2) -0.012(2) C31 0.079(3) 0.090(4) 0.072(3) 0.013(3) 0.033(3) -0.014(3) C32 0.068(3) 0.064(3) 0.070(3) -0.007(2) 0.020(2) 0.001(2) C33 0.050(2) 0.070(3) 0.074(3) 0.009(2) 0.002(2) -0.015(2) C34 0.119(4) 0.055(3) 0.053(3) 0.022(2) -0.027(3) -0.014(3) C35 0.0427(19) 0.0369(18) 0.043(2) 0.0019(15) -0.0030(16) 0.0009(15) C36 0.051(2) 0.051(2) 0.078(3) 0.004(2) -0.004(2) 0.0055(19) C37 0.058(2) 0.046(2) 0.041(2) -0.0041(17) 0.0049(18) 0.0028(18) C38 0.0403(19) 0.042(2) 0.045(2) 0.0025(16) 0.0020(16) -0.0071(15) C39 0.099(4) 0.036(2) 0.088(4) 0.004(2) -0.002(3) 0.000(2) C40 0.059(3) 0.038(2) 0.079(3) -0.010(2) 0.001(2) 0.0025(18) C41 0.087(4) 0.073(3) 0.066(3) 0.023(3) -0.011(3) 0.016(3) C42 0.052(2) 0.063(3) 0.040(2) -0.0149(19) 0.0000(18) -0.0077(19) _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 O1 2.110(2) . ? Yb1 N2 2.263(3) . ? Yb1 N4 2.290(3) . ? Yb1 O3 2.381(2) . ? Yb1 O2 2.455(3) . ? Yb1 N3 2.510(3) . ? Yb1 N1 2.586(3) . ? Yb1 C2 2.794(4) . ? Yb1 C1 2.860(4) . ? Si1 N1 1.737(3) . ? Si1 C19 1.867(4) . ? Si1 C20 1.878(4) . ? Si1 C18 1.878(4) . ? Si2 N3 1.738(3) . ? Si2 C23 1.859(5) . ? Si2 C22 1.870(6) . ? Si2 C21 1.875(6) . ? O1 C24 1.349(4) . ? O2 C41 1.406(5) . ? O2 C39 1.408(5) . ? O3 C40 1.428(5) . ? O3 C42 1.437(4) . ? N1 C1 1.333(4) . ? N2 C1 1.325(5) . ? N2 C3 1.465(6) . ? N3 C2 1.328(5) . ? N4 C2 1.306(5) . ? N4 C5 1.472(5) . ? C1 C6 1.504(5) . ? C2 C12 1.510(6) . ? C3 C4 1.445(9) . ? C3 C4' 1.472(9) . ? C3 H3A 0.974(10) . ? C3 H3B 0.979(10) . ? C4 C5 1.462(10) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4' C5 1.466(10) . ? C4' H3A 1.11(6) . ? C4' H4'A 0.9800 . ? C4' H4'B 0.9800 . ? C5 H5A 0.982(10) . ? C5 H5B 0.982(10) . ? C6 C11 1.380(5) . ? C6 C7 1.393(5) . ? C7 C8 1.373(5) . ? C7 H7 0.9400 . ? C8 C9 1.371(6) . ? C8 H8 0.9400 . ? C9 C10 1.381(7) . ? C9 H9 0.9400 . ? C10 C11 1.376(6) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C17 1.365(9) . ? C12 C13 1.383(9) . ? C13 C14 1.388(7) . ? C13 H13 0.9400 . ? C14 C15 1.344(8) . ? C14 H14 0.9400 . ? C15 C16 1.362(8) . ? C15 H15 0.9400 . ? C16 C17 1.412(7) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C29 1.427(5) . ? C24 C25 1.437(5) . ? C25 C26 1.395(5) . ? C25 C30 1.530(6) . ? C26 C27 1.378(6) . ? C26 H26 0.9400 . ? C27 C28 1.366(6) . ? C27 C34 1.519(6) . ? C28 C29 1.400(5) . ? C28 H28 0.9400 . ? C29 C35 1.529(5) . ? C30 C33 1.524(6) . ? C30 C32 1.532(6) . ? C30 C31 1.543(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 C37 1.536(5) . ? C35 C38 1.537(5) . ? C35 C36 1.542(5) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 C40 1.459(7) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 N2 110.50(13) . . ? O1 Yb1 N4 97.36(11) . . ? N2 Yb1 N4 73.73(11) . . ? O1 Yb1 O3 90.64(9) . . ? N2 Yb1 O3 136.12(10) . . ? N4 Yb1 O3 143.19(10) . . ? O1 Yb1 O2 157.32(9) . . ? N2 Yb1 O2 88.86(13) . . ? N4 Yb1 O2 99.44(11) . . ? O3 Yb1 O2 66.83(9) . . ? O1 Yb1 N3 104.19(10) . . ? N2 Yb1 N3 121.08(12) . . ? N4 Yb1 N3 55.50(11) . . ? O3 Yb1 N3 87.69(9) . . ? O2 Yb1 N3 73.61(10) . . ? O1 Yb1 N1 106.31(9) . . ? N2 Yb1 N1 54.62(10) . . ? N4 Yb1 N1 127.83(10) . . ? O3 Yb1 N1 83.12(9) . . ? O2 Yb1 N1 74.76(9) . . ? N3 Yb1 N1 148.18(10) . . ? O1 Yb1 C2 105.59(11) . . ? N2 Yb1 C2 95.53(12) . . ? N4 Yb1 C2 27.55(11) . . ? O3 Yb1 C2 115.84(10) . . ? O2 Yb1 C2 83.30(11) . . ? N3 Yb1 C2 28.36(11) . . ? N1 Yb1 C2 142.42(11) . . ? O1 Yb1 C1 110.32(9) . . ? N2 Yb1 C1 26.89(10) . . ? N4 Yb1 C1 100.45(11) . . ? O3 Yb1 C1 110.30(10) . . ? O2 Yb1 C1 81.45(10) . . ? N3 Yb1 C1 140.40(11) . . ? N1 Yb1 C1 27.74(9) . . ? C2 Yb1 C1 119.88(12) . . ? N1 Si1 C19 108.63(16) . . ? N1 Si1 C20 115.71(18) . . ? C19 Si1 C20 106.0(2) . . ? N1 Si1 C18 113.68(19) . . ? C19 Si1 C18 106.2(2) . . ? C20 Si1 C18 105.9(2) . . ? N3 Si2 C23 111.10(18) . . ? N3 Si2 C22 113.7(2) . . ? C23 Si2 C22 104.8(3) . . ? N3 Si2 C21 111.2(2) . . ? C23 Si2 C21 105.5(3) . . ? C22 Si2 C21 110.1(4) . . ? C24 O1 Yb1 177.6(2) . . ? C41 O2 C39 115.3(4) . . ? C41 O2 Yb1 122.3(3) . . ? C39 O2 Yb1 115.5(3) . . ? C40 O3 C42 112.4(3) . . ? C40 O3 Yb1 121.0(2) . . ? C42 O3 Yb1 126.1(2) . . ? C1 N1 Si1 124.5(3) . . ? C1 N1 Yb1 87.7(2) . . ? Si1 N1 Yb1 147.69(15) . . ? C1 N2 C3 118.8(3) . . ? C1 N2 Yb1 102.6(2) . . ? C3 N2 Yb1 138.1(3) . . ? C2 N3 Si2 125.6(3) . . ? C2 N3 Yb1 87.8(2) . . ? Si2 N3 Yb1 145.24(17) . . ? C2 N4 C5 123.1(3) . . ? C2 N4 Yb1 98.2(2) . . ? C5 N4 Yb1 136.5(3) . . ? N2 C1 N1 115.1(3) . . ? N2 C1 C6 121.6(3) . . ? N1 C1 C6 123.1(3) . . ? N2 C1 Yb1 50.55(18) . . ? N1 C1 Yb1 64.59(18) . . ? C6 C1 Yb1 172.0(3) . . ? N4 C2 N3 116.8(3) . . ? N4 C2 C12 119.8(4) . . ? N3 C2 C12 123.4(4) . . ? N4 C2 Yb1 54.23(19) . . ? N3 C2 Yb1 63.86(19) . . ? C12 C2 Yb1 166.5(4) . . ? C4 C3 N2 112.3(5) . . ? C4 C3 C4' 45.0(5) . . ? N2 C3 C4' 114.4(5) . . ? C4 C3 H3A 94(4) . . ? N2 C3 H3A 98(4) . . ? C4' C3 H3A 49(4) . . ? C4 C3 H3B 126(3) . . ? N2 C3 H3B 118(3) . . ? C4' C3 H3B 120(3) . . ? H3A C3 H3B 97(5) . . ? C3 C4 C5 120.3(7) . . ? C3 C4 H4A 107.2 . . ? C5 C4 H4A 107.2 . . ? C3 C4 H4B 107.2 . . ? C5 C4 H4B 107.2 . . ? H4A C4 H4B 106.9 . . ? C5 C4' C3 118.3(7) . . ? C5 C4' H3A 138(3) . . ? C3 C4' H3A 41.4(6) . . ? C5 C4' H4'A 107.7 . . ? C3 C4' H4'A 107.7 . . ? H3A C4' H4'A 113.8 . . ? C5 C4' H4'B 107.7 . . ? C3 C4' H4'B 107.7 . . ? H3A C4' H4'B 66.8 . . ? H4'A C4' H4'B 107.1 . . ? C4 C5 C4' 44.8(5) . . ? C4 C5 N4 113.2(4) . . ? C4' C5 N4 112.1(5) . . ? C4 C5 H5A 125(3) . . ? C4' C5 H5A 88(3) . . ? N4 C5 H5A 110(3) . . ? C4 C5 H5B 104(3) . . ? C4' C5 H5B 137(3) . . ? N4 C5 H5B 107(3) . . ? H5A C5 H5B 94(4) . . ? C11 C6 C7 118.3(4) . . ? C11 C6 C1 120.5(3) . . ? C7 C6 C1 121.1(3) . . ? C8 C7 C6 120.5(4) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 119.7(4) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 119.9(4) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C6 121.0(4) . . ? C10 C11 H11 119.5 . . ? C6 C11 H11 119.5 . . ? C17 C12 C13 119.1(5) . . ? C17 C12 C2 121.6(6) . . ? C13 C12 C2 119.2(6) . . ? C12 C13 C14 121.1(7) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 117.5(7) . . ? C15 C14 H14 121.2 . . ? C13 C14 H14 121.2 . . ? C14 C15 C16 124.6(6) . . ? C14 C15 H15 117.7 . . ? C16 C15 H15 117.7 . . ? C15 C16 C17 116.7(6) . . ? C15 C16 H16 121.7 . . ? C17 C16 H16 121.7 . . ? C12 C17 C16 120.8(7) . . ? C12 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O1 C24 C29 120.6(3) . . ? O1 C24 C25 121.0(3) . . ? C29 C24 C25 118.4(3) . . ? C26 C25 C24 118.2(4) . . ? C26 C25 C30 119.2(4) . . ? C24 C25 C30 122.7(3) . . ? C27 C26 C25 123.8(4) . . ? C27 C26 H26 118.1 . . ? C25 C26 H26 118.1 . . ? C28 C27 C26 117.5(4) . . ? C28 C27 C34 121.1(4) . . ? C26 C27 C34 121.5(4) . . ? C27 C28 C29 123.5(4) . . ? C27 C28 H28 118.3 . . ? C29 C28 H28 118.3 . . ? C28 C29 C24 118.7(3) . . ? C28 C29 C35 119.1(3) . . ? C24 C29 C35 122.2(3) . . ? C33 C30 C25 110.0(4) . . ? C33 C30 C32 110.8(4) . . ? C25 C30 C32 109.8(3) . . ? C33 C30 C31 106.9(4) . . ? C25 C30 C31 112.5(4) . . ? C32 C30 C31 106.7(4) . . ? 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 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C27 C34 H34A 109.5 . . ? C27 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C27 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C29 C35 C37 110.5(3) . . ? C29 C35 C38 109.8(3) . . ? C37 C35 C38 111.2(3) . . ? C29 C35 C36 112.7(3) . . ? C37 C35 C36 107.0(3) . . ? C38 C35 C36 105.5(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O2 C39 C40 112.9(4) . . ? O2 C39 H39A 109.0 . . ? C40 C39 H39A 109.0 . . ? O2 C39 H39B 109.0 . . ? C40 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? O3 C40 C39 110.3(4) . . ? O3 C40 H40A 109.6 . . ? C39 C40 H40A 109.6 . . ? O3 C40 H40B 109.6 . . ? C39 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? O2 C41 H41A 109.5 . . ? O2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O3 C42 H42A 109.5 . . ? O3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 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 N2 Yb1 O1 C24 -9(5) . . . . ? N4 Yb1 O1 C24 -84(5) . . . . ? O3 Yb1 O1 C24 132(5) . . . . ? O2 Yb1 O1 C24 138(5) . . . . ? N3 Yb1 O1 C24 -141(5) . . . . ? N1 Yb1 O1 C24 49(5) . . . . ? C2 Yb1 O1 C24 -111(5) . . . . ? C1 Yb1 O1 C24 20(5) . . . . ? O1 Yb1 O2 C41 -174.0(3) . . . . ? N2 Yb1 O2 C41 -24.6(3) . . . . ? N4 Yb1 O2 C41 48.7(3) . . . . ? O3 Yb1 O2 C41 -167.0(3) . . . . ? N3 Yb1 O2 C41 98.4(3) . . . . ? N1 Yb1 O2 C41 -78.1(3) . . . . ? C2 Yb1 O2 C41 71.1(3) . . . . ? C1 Yb1 O2 C41 -50.6(3) . . . . ? O1 Yb1 O2 C39 -24.4(4) . . . . ? N2 Yb1 O2 C39 125.0(3) . . . . ? N4 Yb1 O2 C39 -161.7(3) . . . . ? O3 Yb1 O2 C39 -17.5(3) . . . . ? N3 Yb1 O2 C39 -112.1(3) . . . . ? N1 Yb1 O2 C39 71.5(3) . . . . ? C2 Yb1 O2 C39 -139.3(3) . . . . ? C1 Yb1 O2 C39 99.0(3) . . . . ? O1 Yb1 O3 C40 172.0(3) . . . . ? N2 Yb1 O3 C40 -66.8(3) . . . . ? N4 Yb1 O3 C40 68.8(3) . . . . ? O2 Yb1 O3 C40 -5.3(3) . . . . ? N3 Yb1 O3 C40 67.9(3) . . . . ? N1 Yb1 O3 C40 -81.6(3) . . . . ? C2 Yb1 O3 C40 64.3(3) . . . . ? C1 Yb1 O3 C40 -76.0(3) . . . . ? O1 Yb1 O3 C42 0.8(3) . . . . ? N2 Yb1 O3 C42 121.9(3) . . . . ? N4 Yb1 O3 C42 -102.5(3) . . . . ? O2 Yb1 O3 C42 -176.5(3) . . . . ? N3 Yb1 O3 C42 -103.4(3) . . . . ? N1 Yb1 O3 C42 107.1(3) . . . . ? C2 Yb1 O3 C42 -106.9(3) . . . . ? C1 Yb1 O3 C42 112.8(3) . . . . ? C19 Si1 N1 C1 172.4(3) . . . . ? C20 Si1 N1 C1 53.3(4) . . . . ? C18 Si1 N1 C1 -69.5(4) . . . . ? C19 Si1 N1 Yb1 -14.0(3) . . . . ? C20 Si1 N1 Yb1 -133.1(3) . . . . ? C18 Si1 N1 Yb1 104.1(3) . . . . ? O1 Yb1 N1 C1 -102.8(2) . . . . ? N2 Yb1 N1 C1 1.1(2) . . . . ? N4 Yb1 N1 C1 10.6(2) . . . . ? O3 Yb1 N1 C1 168.6(2) . . . . ? O2 Yb1 N1 C1 100.8(2) . . . . ? N3 Yb1 N1 C1 94.3(3) . . . . ? C2 Yb1 N1 C1 44.3(3) . . . . ? O1 Yb1 N1 Si1 82.5(3) . . . . ? N2 Yb1 N1 Si1 -173.6(4) . . . . ? N4 Yb1 N1 Si1 -164.2(3) . . . . ? O3 Yb1 N1 Si1 -6.2(3) . . . . ? O2 Yb1 N1 Si1 -74.0(3) . . . . ? N3 Yb1 N1 Si1 -80.4(3) . . . . ? C2 Yb1 N1 Si1 -130.4(3) . . . . ? C1 Yb1 N1 Si1 -174.7(4) . . . . ? O1 Yb1 N2 C1 94.7(3) . . . . ? N4 Yb1 N2 C1 -173.3(3) . . . . ? O3 Yb1 N2 C1 -19.2(4) . . . . ? O2 Yb1 N2 C1 -73.2(3) . . . . ? N3 Yb1 N2 C1 -143.2(2) . . . . ? N1 Yb1 N2 C1 -1.1(2) . . . . ? C2 Yb1 N2 C1 -156.3(3) . . . . ? O1 Yb1 N2 C3 -75.6(6) . . . . ? N4 Yb1 N2 C3 16.3(6) . . . . ? O3 Yb1 N2 C3 170.4(5) . . . . ? O2 Yb1 N2 C3 116.5(6) . . . . ? N3 Yb1 N2 C3 46.4(6) . . . . ? N1 Yb1 N2 C3 -171.5(6) . . . . ? C2 Yb1 N2 C3 33.3(6) . . . . ? C1 Yb1 N2 C3 -170.4(8) . . . . ? C23 Si2 N3 C2 -161.8(4) . . . . ? C22 Si2 N3 C2 -43.8(5) . . . . ? C21 Si2 N3 C2 81.0(4) . . . . ? C23 Si2 N3 Yb1 36.6(4) . . . . ? C22 Si2 N3 Yb1 154.5(4) . . . . ? C21 Si2 N3 Yb1 -80.6(4) . . . . ? O1 Yb1 N3 C2 96.6(2) . . . . ? N2 Yb1 N3 C2 -28.4(3) . . . . ? N4 Yb1 N3 C2 7.4(2) . . . . ? O3 Yb1 N3 C2 -173.3(2) . . . . ? O2 Yb1 N3 C2 -106.8(3) . . . . ? N1 Yb1 N3 C2 -100.3(3) . . . . ? C1 Yb1 N3 C2 -53.6(3) . . . . ? O1 Yb1 N3 Si2 -98.2(3) . . . . ? N2 Yb1 N3 Si2 136.7(3) . . . . ? N4 Yb1 N3 Si2 172.5(4) . . . . ? O3 Yb1 N3 Si2 -8.2(3) . . . . ? O2 Yb1 N3 Si2 58.4(3) . . . . ? N1 Yb1 N3 Si2 64.8(4) . . . . ? C2 Yb1 N3 Si2 165.1(5) . . . . ? C1 Yb1 N3 Si2 111.6(3) . . . . ? O1 Yb1 N4 C2 -109.8(3) . . . . ? N2 Yb1 N4 C2 140.9(3) . . . . ? O3 Yb1 N4 C2 -8.7(4) . . . . ? O2 Yb1 N4 C2 54.9(3) . . . . ? N3 Yb1 N4 C2 -7.6(2) . . . . ? N1 Yb1 N4 C2 132.9(2) . . . . ? C1 Yb1 N4 C2 137.9(3) . . . . ? O1 Yb1 N4 C5 87.8(5) . . . . ? N2 Yb1 N4 C5 -21.5(5) . . . . ? O3 Yb1 N4 C5 -171.2(4) . . . . ? O2 Yb1 N4 C5 -107.5(5) . . . . ? N3 Yb1 N4 C5 -170.1(5) . . . . ? N1 Yb1 N4 C5 -29.5(5) . . . . ? C2 Yb1 N4 C5 -162.5(6) . . . . ? C1 Yb1 N4 C5 -24.6(5) . . . . ? C3 N2 C1 N1 174.6(4) . . . . ? Yb1 N2 C1 N1 2.0(4) . . . . ? C3 N2 C1 C6 -9.1(7) . . . . ? Yb1 N2 C1 C6 178.2(3) . . . . ? C3 N2 C1 Yb1 172.7(6) . . . . ? Si1 N1 C1 N2 174.9(3) . . . . ? Yb1 N1 C1 N2 -1.7(3) . . . . ? Si1 N1 C1 C6 -1.3(5) . . . . ? Yb1 N1 C1 C6 -177.9(3) . . . . ? Si1 N1 C1 Yb1 176.6(3) . . . . ? O1 Yb1 C1 N2 -95.5(3) . . . . ? N4 Yb1 C1 N2 6.5(3) . . . . ? O3 Yb1 C1 N2 165.9(3) . . . . ? O2 Yb1 C1 N2 104.6(3) . . . . ? N3 Yb1 C1 N2 53.6(3) . . . . ? N1 Yb1 C1 N2 178.0(4) . . . . ? C2 Yb1 C1 N2 27.5(3) . . . . ? O1 Yb1 C1 N1 86.5(2) . . . . ? N2 Yb1 C1 N1 -178.0(4) . . . . ? N4 Yb1 C1 N1 -171.5(2) . . . . ? O3 Yb1 C1 N1 -12.1(2) . . . . ? O2 Yb1 C1 N1 -73.4(2) . . . . ? N3 Yb1 C1 N1 -124.4(2) . . . . ? C2 Yb1 C1 N1 -150.6(2) . . . . ? O1 Yb1 C1 C6 -106.4(18) . . . . ? N2 Yb1 C1 C6 -10.9(17) . . . . ? N4 Yb1 C1 C6 -4.4(18) . . . . ? O3 Yb1 C1 C6 155.0(18) . . . . ? O2 Yb1 C1 C6 93.7(18) . . . . ? N3 Yb1 C1 C6 42.7(18) . . . . ? N1 Yb1 C1 C6 167.1(19) . . . . ? C2 Yb1 C1 C6 16.5(18) . . . . ? C5 N4 C2 N3 179.0(4) . . . . ? Yb1 N4 C2 N3 13.3(4) . . . . ? C5 N4 C2 C12 0.1(7) . . . . ? Yb1 N4 C2 C12 -165.6(4) . . . . ? C5 N4 C2 Yb1 165.7(5) . . . . ? Si2 N3 C2 N4 178.3(3) . . . . ? Yb1 N3 C2 N4 -12.0(4) . . . . ? Si2 N3 C2 C12 -2.8(7) . . . . ? Yb1 N3 C2 C12 166.8(5) . . . . ? Si2 N3 C2 Yb1 -169.6(3) . . . . ? O1 Yb1 C2 N4 75.7(3) . . . . ? N2 Yb1 C2 N4 -37.4(3) . . . . ? O3 Yb1 C2 N4 174.2(3) . . . . ? O2 Yb1 C2 N4 -125.6(3) . . . . ? N3 Yb1 C2 N4 166.7(4) . . . . ? N1 Yb1 C2 N4 -71.5(3) . . . . ? C1 Yb1 C2 N4 -49.5(3) . . . . ? O1 Yb1 C2 N3 -91.1(2) . . . . ? N2 Yb1 C2 N3 155.8(3) . . . . ? N4 Yb1 C2 N3 -166.7(4) . . . . ? O3 Yb1 C2 N3 7.4(3) . . . . ? O2 Yb1 C2 N3 67.6(2) . . . . ? N1 Yb1 C2 N3 121.7(2) . . . . ? C1 Yb1 C2 N3 143.7(2) . . . . ? O1 Yb1 C2 C12 143.5(15) . . . . ? N2 Yb1 C2 C12 30.4(15) . . . . ? N4 Yb1 C2 C12 67.8(15) . . . . ? O3 Yb1 C2 C12 -118.0(15) . . . . ? O2 Yb1 C2 C12 -57.8(15) . . . . ? N3 Yb1 C2 C12 -125.5(16) . . . . ? N1 Yb1 C2 C12 -3.7(16) . . . . ? C1 Yb1 C2 C12 18.3(16) . . . . ? C1 N2 C3 C4 -155.2(6) . . . . ? Yb1 N2 C3 C4 14.0(10) . . . . ? C1 N2 C3 C4' 155.6(6) . . . . ? Yb1 N2 C3 C4' -35.2(10) . . . . ? N2 C3 C4 C5 -56.9(10) . . . . ? C4' C3 C4 C5 45.8(7) . . . . ? C4 C3 C4' C5 -44.5(7) . . . . ? N2 C3 C4' C5 53.3(10) . . . . ? C3 C4 C5 C4' -46.2(7) . . . . ? C3 C4 C5 N4 52.4(9) . . . . ? C3 C4' C5 C4 44.0(7) . . . . ? C3 C4' C5 N4 -57.2(9) . . . . ? C2 N4 C5 C4 -163.0(6) . . . . ? Yb1 N4 C5 C4 -3.9(8) . . . . ? C2 N4 C5 C4' -114.3(6) . . . . ? Yb1 N4 C5 C4' 44.9(8) . . . . ? N2 C1 C6 C11 -88.6(5) . . . . ? N1 C1 C6 C11 87.3(5) . . . . ? Yb1 C1 C6 C11 -78.7(18) . . . . ? N2 C1 C6 C7 90.1(5) . . . . ? N1 C1 C6 C7 -93.9(5) . . . . ? Yb1 C1 C6 C7 100.0(18) . . . . ? C11 C6 C7 C8 -2.6(6) . . . . ? C1 C6 C7 C8 178.7(4) . . . . ? C6 C7 C8 C9 1.3(7) . . . . ? C7 C8 C9 C10 0.7(8) . . . . ? C8 C9 C10 C11 -1.4(8) . . . . ? C9 C10 C11 C6 0.0(8) . . . . ? C7 C6 C11 C10 1.9(7) . . . . ? C1 C6 C11 C10 -179.3(4) . . . . ? N4 C2 C12 C17 -77.3(7) . . . . ? N3 C2 C12 C17 103.9(7) . . . . ? Yb1 C2 C12 C17 -137.2(13) . . . . ? N4 C2 C12 C13 99.5(7) . . . . ? N3 C2 C12 C13 -79.3(7) . . . . ? Yb1 C2 C12 C13 39.6(19) . . . . ? C17 C12 C13 C14 -1.7(10) . . . . ? C2 C12 C13 C14 -178.6(5) . . . . ? C12 C13 C14 C15 -1.0(10) . . . . ? C13 C14 C15 C16 2.6(10) . . . . ? C14 C15 C16 C17 -1.5(10) . . . . ? C13 C12 C17 C16 2.9(10) . . . . ? C2 C12 C17 C16 179.7(5) . . . . ? C15 C16 C17 C12 -1.4(9) . . . . ? Yb1 O1 C24 C29 -39(5) . . . . ? Yb1 O1 C24 C25 142(5) . . . . ? O1 C24 C25 C26 177.8(3) . . . . ? C29 C24 C25 C26 -1.8(5) . . . . ? O1 C24 C25 C30 -2.5(5) . . . . ? C29 C24 C25 C30 177.9(3) . . . . ? C24 C25 C26 C27 1.2(6) . . . . ? C30 C25 C26 C27 -178.5(4) . . . . ? C25 C26 C27 C28 0.5(6) . . . . ? C25 C26 C27 C34 -178.6(4) . . . . ? C26 C27 C28 C29 -1.6(6) . . . . ? C34 C27 C28 C29 177.6(4) . . . . ? C27 C28 C29 C24 0.9(5) . . . . ? C27 C28 C29 C35 -177.8(3) . . . . ? O1 C24 C29 C28 -178.8(3) . . . . ? C25 C24 C29 C28 0.8(5) . . . . ? O1 C24 C29 C35 -0.1(5) . . . . ? C25 C24 C29 C35 179.5(3) . . . . ? C26 C25 C30 C33 118.8(4) . . . . ? C24 C25 C30 C33 -60.9(5) . . . . ? C26 C25 C30 C32 -119.0(4) . . . . ? C24 C25 C30 C32 61.3(5) . . . . ? C26 C25 C30 C31 -0.3(5) . . . . ? C24 C25 C30 C31 180.0(4) . . . . ? C28 C29 C35 C37 -118.5(4) . . . . ? C24 C29 C35 C37 62.8(4) . . . . ? C28 C29 C35 C38 118.5(4) . . . . ? C24 C29 C35 C38 -60.1(4) . . . . ? C28 C29 C35 C36 1.2(5) . . . . ? C24 C29 C35 C36 -177.5(3) . . . . ? C41 O2 C39 C40 -170.5(4) . . . . ? Yb1 O2 C39 C40 37.8(5) . . . . ? C42 O3 C40 C39 -161.9(4) . . . . ? Yb1 O3 C40 C39 25.8(5) . . . . ? O2 C39 C40 O3 -40.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.553 _refine_diff_density_min -0.930 _refine_diff_density_rms 0.080