# PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Dr. Yingming Yao' _publ_contact_author_email 'yaoym@suda.edu.cn' _publ_contact_author_fax '86-512-65880305' _publ_contact_author_phone '86-512-65882806' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'Inorg. Chem.' _publ_requested_category 'FM' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of Rare-Earth Metal Amides Bearing an Imidazolidine-Bridged Bis(phenolato) Ligand and Their Application in the Polymerization of L-Lactide ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Zhongjian Zhang' ; College of Chemistry, Chemical Engineering and Materials Science Dushu Lake Campus Soochow University Suzhou, 215123 P. R. China ; 'Xiaoping Xu' ; College of Chemistry, Chemical Engineering and Materials Science Dushu Lake Campus Soochow University Suzhou, 215123 P. R. China ; 'Wenyi Li' ; College of Chemistry, Chemical Engineering and Materials Science Dushu Lake Campus Soochow University Suzhou, 215123 P. R. China ; 'Yingming Yao' ; College of Chemistry, Chemical Engineering and Materials Science Dushu Lake Campus Soochow University Suzhou, 215123 P. R. China ; 'Yong Zhang' ; College of Chemistry, Chemical Engineering and Materials Science Dushu Lake Campus Soochow University Suzhou, 215123 P. R. China ; 'Qi Shen' ; College of Chemistry, Chemical Engineering and Materials Science Dushu Lake Campus Soochow University Suzhou, 215123 P. R. China ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data_complex1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H76 La N3 O3 Si2' _chemical_formula_sum 'C43 H76 La N3 O3 Si2' _chemical_formula_weight 878.16 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' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 10.3838(12) _cell_length_b 20.663(2) _cell_length_c 22.752(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.223(3) _cell_angle_gamma 90.00 _cell_volume 4804.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14580 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.35 _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 1856 _exptl_absorpt_coefficient_mu 0.976 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5921 _exptl_absorpt_correction_T_max 0.7584 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22563 _diffrn_reflns_av_R_equivalents 0.0967 _diffrn_reflns_av_sigmaI/netI 0.1370 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8754 _reflns_number_gt 5679 _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 ? _computing_publication_material ? _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^)+(0.1103P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8754 _refine_ls_number_parameters 480 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1512 _refine_ls_R_factor_gt 0.0961 _refine_ls_wR_factor_ref 0.2408 _refine_ls_wR_factor_gt 0.2097 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.109 _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 La1 La 0.39556(5) 0.51175(2) 0.28958(2) 0.0369(2) Uani 1 1 d . . . Si1 Si 0.5737(3) 0.37801(15) 0.24566(16) 0.0610(8) Uani 1 1 d . . . Si2 Si 0.6346(3) 0.41153(16) 0.37678(15) 0.0594(8) Uani 1 1 d . . . O1 O 0.3651(6) 0.5841(3) 0.3609(3) 0.0487(17) Uani 1 1 d . . . O2 O 0.2778(6) 0.5415(3) 0.2010(3) 0.0516(17) Uani 1 1 d . . . O3 O 0.5937(7) 0.5799(4) 0.2670(3) 0.066(2) Uani 1 1 d D . . N1 N 0.2172(7) 0.4670(3) 0.3526(3) 0.0367(17) Uani 1 1 d . . . N2 N 0.1793(6) 0.4362(3) 0.2596(3) 0.0383(18) Uani 1 1 d . . . N3 N 0.5496(7) 0.4227(3) 0.3057(3) 0.0447(19) Uani 1 1 d . . . C1 C 0.2759(8) 0.6099(4) 0.3891(4) 0.036(2) Uani 1 1 d . . . C2 C 0.2742(8) 0.6777(4) 0.4028(4) 0.041(2) Uani 1 1 d . . . C3 C 0.1710(8) 0.7012(5) 0.4270(4) 0.045(2) Uani 1 1 d . . . H3 H 0.1686 0.7456 0.4338 0.053 Uiso 1 1 calc R . . C4 C 0.0698(8) 0.6639(4) 0.4420(4) 0.041(2) Uani 1 1 d . . . C5 C 0.0789(8) 0.5975(5) 0.4315(4) 0.045(2) Uani 1 1 d . . . H5 H 0.0148 0.5702 0.4414 0.055 Uiso 1 1 calc R . . C6 C 0.1796(8) 0.5705(5) 0.4067(4) 0.043(2) Uani 1 1 d . . . C7 C 0.1618(9) 0.5433(4) 0.1636(4) 0.041(2) Uani 1 1 d . . . C8 C 0.1255(8) 0.5957(4) 0.1240(4) 0.042(2) Uani 1 1 d . . . C9 C 0.0009(9) 0.5935(5) 0.0872(4) 0.049(3) Uani 1 1 d . . . H9 H -0.0223 0.6275 0.0606 0.059 Uiso 1 1 calc R . . C10 C -0.0899(9) 0.5437(5) 0.0878(4) 0.045(2) Uani 1 1 d . . . C11 C -0.0494(9) 0.4931(4) 0.1268(5) 0.047(2) Uani 1 1 d . . . H11 H -0.1068 0.4588 0.1284 0.057 Uiso 1 1 calc R . . C12 C 0.0737(8) 0.4910(4) 0.1640(4) 0.037(2) Uani 1 1 d . . . C13 C 0.1895(9) 0.4980(4) 0.4082(4) 0.042(2) Uani 1 1 d . . . H13A H 0.2581 0.4858 0.4410 0.051 Uiso 1 1 calc R . . H13B H 0.1079 0.4807 0.4166 0.051 Uiso 1 1 calc R . . C14 C 0.1228(8) 0.4784(4) 0.2979(4) 0.039(2) Uani 1 1 d . . . H14A H 0.0350 0.4653 0.3017 0.047 Uiso 1 1 calc R . . H14B H 0.1223 0.5232 0.2850 0.047 Uiso 1 1 calc R . . C15 C 0.2215(9) 0.3951(4) 0.3569(4) 0.044(2) Uani 1 1 d . . . H15A H 0.1546 0.3788 0.3778 0.053 Uiso 1 1 calc R . . H15B H 0.3065 0.3802 0.3771 0.053 Uiso 1 1 calc R . . C16 C 0.1958(9) 0.3747(4) 0.2926(4) 0.047(2) Uani 1 1 d . . . H16A H 0.2689 0.3503 0.2828 0.056 Uiso 1 1 calc R . . H16B H 0.1172 0.3485 0.2836 0.056 Uiso 1 1 calc R . . C17 C 0.1100(9) 0.4293(4) 0.1976(4) 0.049(3) Uani 1 1 d . . . H17A H 0.0305 0.4048 0.1981 0.059 Uiso 1 1 calc R . . H17B H 0.1644 0.4040 0.1758 0.059 Uiso 1 1 calc R . . C18 C 0.3859(8) 0.7220(4) 0.3928(4) 0.044(2) Uani 1 1 d . . . C19 C 0.3726(10) 0.7909(4) 0.4167(5) 0.059(3) Uani 1 1 d . . . H19A H 0.4381 0.8183 0.4048 0.088 Uiso 1 1 calc R . . H19B H 0.3840 0.7897 0.4595 0.088 Uiso 1 1 calc R . . H19C H 0.2873 0.8076 0.4007 0.088 Uiso 1 1 calc R . . C20 C 0.3913(12) 0.7276(6) 0.3275(5) 0.073(3) Uani 1 1 d . . . H20A H 0.3995 0.6853 0.3112 0.110 Uiso 1 1 calc R . . H20B H 0.4653 0.7535 0.3224 0.110 Uiso 1 1 calc R . . H20C H 0.3125 0.7477 0.3071 0.110 Uiso 1 1 calc R . . C21 C 0.5179(9) 0.6955(5) 0.4269(5) 0.068(3) Uani 1 1 d . . . H21A H 0.5327 0.6529 0.4125 0.102 Uiso 1 1 calc R . . H21B H 0.5150 0.6934 0.4688 0.102 Uiso 1 1 calc R . . H21C H 0.5876 0.7237 0.4206 0.102 Uiso 1 1 calc R . . C22 C -0.0389(9) 0.6942(5) 0.4684(5) 0.050(3) Uani 1 1 d . . . C23 C -0.1051(12) 0.7481(6) 0.4290(6) 0.092(4) Uani 1 1 d . . . H23A H -0.1567 0.7298 0.3937 0.138 Uiso 1 1 calc R . . H23B H -0.0398 0.7762 0.4178 0.138 Uiso 1 1 calc R . . H23C H -0.1606 0.7723 0.4504 0.138 Uiso 1 1 calc R . . C24 C 0.0196(11) 0.7240(6) 0.5304(6) 0.077(4) Uani 1 1 d . . . H24A H -0.0479 0.7465 0.5460 0.115 Uiso 1 1 calc R . . H24B H 0.0881 0.7538 0.5259 0.115 Uiso 1 1 calc R . . H24C H 0.0546 0.6901 0.5575 0.115 Uiso 1 1 calc R . . C25 C -0.1427(10) 0.6463(6) 0.4799(6) 0.072(3) Uani 1 1 d . . . H25A H -0.1746 0.6226 0.4440 0.108 Uiso 1 1 calc R . . H25B H -0.2137 0.6693 0.4922 0.108 Uiso 1 1 calc R . . H25C H -0.1052 0.6168 0.5108 0.108 Uiso 1 1 calc R . . C26 C 0.2217(9) 0.6507(5) 0.1187(5) 0.051(3) Uani 1 1 d . . . C27 C 0.1632(12) 0.7002(6) 0.0702(6) 0.087(4) Uani 1 1 d . . . H27A H 0.2225 0.7359 0.0705 0.130 Uiso 1 1 calc R . . H27B H 0.0810 0.7158 0.0783 0.130 Uiso 1 1 calc R . . H27C H 0.1498 0.6797 0.0317 0.130 Uiso 1 1 calc R . . C28 C 0.3432(10) 0.6245(6) 0.0994(6) 0.080(4) Uani 1 1 d . . . H28A H 0.3789 0.5902 0.1258 0.120 Uiso 1 1 calc R . . H28B H 0.4067 0.6585 0.1008 0.120 Uiso 1 1 calc R . . H28C H 0.3213 0.6082 0.0594 0.120 Uiso 1 1 calc R . . C29 C 0.2528(13) 0.6871(5) 0.1780(6) 0.082(4) Uani 1 1 d . . . H29A H 0.2910 0.6578 0.2090 0.123 Uiso 1 1 calc R . . H29B H 0.1736 0.7049 0.1875 0.123 Uiso 1 1 calc R . . H29C H 0.3133 0.7215 0.1746 0.123 Uiso 1 1 calc R . . C30 C -0.2199(9) 0.5445(6) 0.0436(5) 0.061(3) Uani 1 1 d . . . C31 C -0.2914(11) 0.6086(7) 0.0512(6) 0.107(5) Uani 1 1 d . . . H31A H -0.2381 0.6444 0.0431 0.160 Uiso 1 1 calc R . . H31B H -0.3075 0.6118 0.0913 0.160 Uiso 1 1 calc R . . H31C H -0.3731 0.6096 0.0238 0.160 Uiso 1 1 calc R . . C32 C -0.3078(12) 0.4887(7) 0.0553(7) 0.110(6) Uani 1 1 d . . . H32A H -0.3938 0.4948 0.0323 0.165 Uiso 1 1 calc R . . H32B H -0.3128 0.4874 0.0970 0.165 Uiso 1 1 calc R . . H32C H -0.2722 0.4487 0.0439 0.165 Uiso 1 1 calc R . . C33 C -0.1936(12) 0.5404(6) -0.0199(5) 0.076(3) Uani 1 1 d . . . H33A H -0.1430 0.5024 -0.0240 0.113 Uiso 1 1 calc R . . H33B H -0.1460 0.5781 -0.0284 0.113 Uiso 1 1 calc R . . H33C H -0.2753 0.5383 -0.0473 0.113 Uiso 1 1 calc R . . C34 C 0.5138(14) 0.2923(6) 0.2463(7) 0.105(5) Uani 1 1 d . . . H34A H 0.5651 0.2693 0.2790 0.158 Uiso 1 1 calc R . . H34B H 0.5220 0.2715 0.2094 0.158 Uiso 1 1 calc R . . H34C H 0.4236 0.2922 0.2508 0.158 Uiso 1 1 calc R . . C35 C 0.7467(11) 0.3736(7) 0.2330(7) 0.104(5) Uani 1 1 d . . . H35A H 0.7833 0.4163 0.2346 0.156 Uiso 1 1 calc R . . H35B H 0.7484 0.3549 0.1945 0.156 Uiso 1 1 calc R . . H35C H 0.7972 0.3472 0.2634 0.156 Uiso 1 1 calc R . . C36 C 0.4801(13) 0.4133(7) 0.1747(5) 0.093(4) Uani 1 1 d . . . H36A H 0.3887 0.4152 0.1771 0.140 Uiso 1 1 calc R . . H36B H 0.4920 0.3867 0.1416 0.140 Uiso 1 1 calc R . . H36C H 0.5116 0.4562 0.1693 0.140 Uiso 1 1 calc R . . C37 C 0.8142(11) 0.4320(7) 0.3866(7) 0.102(5) Uani 1 1 d . . . H37A H 0.8572 0.4016 0.3647 0.152 Uiso 1 1 calc R . . H37B H 0.8524 0.4299 0.4282 0.152 Uiso 1 1 calc R . . H37C H 0.8244 0.4749 0.3719 0.152 Uiso 1 1 calc R . . C38 C 0.5710(14) 0.4653(8) 0.4291(6) 0.105(5) Uani 1 1 d . . . H38A H 0.5640 0.5085 0.4133 0.158 Uiso 1 1 calc R . . H38B H 0.6295 0.4650 0.4668 0.158 Uiso 1 1 calc R . . H38C H 0.4862 0.4505 0.4345 0.158 Uiso 1 1 calc R . . C39 C 0.6225(13) 0.3290(7) 0.4063(7) 0.108(6) Uani 1 1 d . . . H39A H 0.5320 0.3171 0.4026 0.163 Uiso 1 1 calc R . . H39B H 0.6631 0.3278 0.4476 0.163 Uiso 1 1 calc R . . H39C H 0.6660 0.2991 0.3840 0.163 Uiso 1 1 calc R . . C40 C 0.624(3) 0.6117(16) 0.2140(10) 0.116(8) Uiso 0.50 1 d PD . . C40' C 0.673(3) 0.5634(16) 0.2217(13) 0.116(8) Uiso 0.50 1 d PD . . C41 C 0.749(3) 0.6481(13) 0.2331(13) 0.093(6) Uiso 0.50 1 d PD . . C41' C 0.795(3) 0.6031(14) 0.2284(12) 0.093(6) Uiso 0.50 1 d PD . . C42 C 0.812(3) 0.5955(16) 0.2751(16) 0.123(8) Uiso 0.50 1 d PD . . C42' C 0.809(3) 0.6268(17) 0.2918(13) 0.123(8) Uiso 0.50 1 d PD . . C43 C 0.708(4) 0.5884(19) 0.3147(17) 0.135(10) Uiso 0.50 1 d PD . . C43' C 0.673(3) 0.6242(16) 0.3079(15) 0.135(10) Uiso 0.50 1 d PD . . 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 La1 0.0305(3) 0.0375(3) 0.0422(4) -0.0002(3) 0.0045(2) 0.0008(2) Si1 0.0511(17) 0.0582(18) 0.076(2) -0.0039(17) 0.0171(16) 0.0089(14) Si2 0.0398(15) 0.069(2) 0.066(2) 0.0099(16) 0.0005(14) 0.0029(14) O1 0.047(4) 0.044(4) 0.060(4) -0.016(3) 0.022(3) -0.004(3) O2 0.047(4) 0.048(4) 0.054(4) 0.009(3) -0.006(3) -0.007(3) O3 0.056(4) 0.076(5) 0.065(5) -0.003(4) 0.010(4) -0.024(4) N1 0.042(4) 0.031(4) 0.037(4) 0.002(3) 0.007(3) 0.003(3) N2 0.034(4) 0.030(4) 0.050(5) -0.004(3) 0.006(4) -0.006(3) N3 0.041(4) 0.045(5) 0.044(5) 0.010(4) -0.005(4) 0.008(3) C1 0.025(4) 0.041(5) 0.044(6) -0.002(4) 0.008(4) -0.009(4) C2 0.043(5) 0.028(5) 0.050(6) -0.001(4) 0.002(4) -0.006(4) C3 0.039(5) 0.043(5) 0.052(6) 0.002(5) 0.011(5) 0.000(4) C4 0.032(4) 0.051(6) 0.041(6) 0.001(4) 0.007(4) 0.003(4) C5 0.035(5) 0.053(6) 0.051(6) -0.001(5) 0.014(4) -0.003(4) C6 0.039(5) 0.052(6) 0.037(5) 0.000(4) 0.006(4) 0.004(4) C7 0.045(5) 0.044(5) 0.033(5) 0.001(4) 0.004(4) 0.004(4) C8 0.045(5) 0.031(5) 0.048(6) 0.000(4) 0.008(5) 0.002(4) C9 0.044(5) 0.048(6) 0.052(6) 0.012(5) -0.002(5) 0.012(4) C10 0.048(5) 0.044(6) 0.041(6) 0.008(5) 0.002(5) 0.000(5) C11 0.043(5) 0.048(6) 0.050(6) -0.018(5) 0.004(5) -0.011(4) C12 0.036(5) 0.048(5) 0.025(5) -0.001(4) 0.001(4) -0.006(4) C13 0.048(5) 0.033(5) 0.045(6) 0.004(4) 0.006(5) -0.006(4) C14 0.032(4) 0.039(5) 0.042(6) 0.009(4) -0.003(4) 0.002(4) C15 0.049(5) 0.031(5) 0.049(6) 0.006(4) 0.002(5) -0.004(4) C16 0.052(6) 0.029(5) 0.059(7) 0.008(5) 0.008(5) 0.005(4) C17 0.056(6) 0.039(5) 0.046(6) 0.005(4) -0.008(5) -0.009(4) C18 0.042(5) 0.029(5) 0.060(7) -0.004(4) 0.010(5) 0.000(4) C19 0.063(6) 0.032(5) 0.081(8) -0.003(5) 0.013(6) -0.006(5) C20 0.094(9) 0.074(8) 0.058(8) -0.011(6) 0.031(7) -0.019(7) C21 0.036(5) 0.065(7) 0.097(9) -0.002(7) -0.002(6) -0.017(5) C22 0.039(5) 0.048(6) 0.062(7) -0.001(5) 0.010(5) 0.007(4) C23 0.067(8) 0.094(10) 0.121(12) 0.040(9) 0.036(8) 0.024(7) C24 0.059(7) 0.090(9) 0.085(9) -0.023(7) 0.022(7) 0.016(6) C25 0.058(7) 0.079(8) 0.086(9) 0.010(7) 0.030(7) 0.010(6) C26 0.055(6) 0.045(6) 0.052(6) 0.012(5) 0.010(5) -0.004(5) C27 0.079(8) 0.067(8) 0.108(11) 0.045(8) 0.001(8) -0.005(6) C28 0.051(7) 0.081(9) 0.108(10) 0.034(8) 0.013(7) -0.002(6) C29 0.096(9) 0.046(7) 0.100(10) -0.014(7) 0.007(8) -0.016(6) C30 0.031(5) 0.099(9) 0.051(7) 0.006(6) 0.002(5) 0.006(5) C31 0.059(7) 0.154(14) 0.096(11) -0.007(10) -0.016(7) 0.063(9) C32 0.048(7) 0.149(14) 0.116(13) 0.045(10) -0.031(8) -0.023(8) C33 0.077(8) 0.085(9) 0.063(8) -0.007(7) 0.006(7) 0.018(7) C34 0.117(12) 0.065(8) 0.140(14) -0.018(9) 0.037(10) 0.009(8) C35 0.062(8) 0.142(13) 0.120(13) -0.014(10) 0.049(9) 0.014(8) C36 0.089(10) 0.123(12) 0.064(9) -0.011(8) 0.006(7) 0.015(9) C37 0.051(7) 0.099(10) 0.140(13) 0.049(10) -0.024(8) -0.002(7) C38 0.094(10) 0.140(13) 0.068(9) -0.030(9) -0.022(8) 0.022(10) C39 0.082(9) 0.106(11) 0.126(13) 0.072(10) -0.012(9) -0.021(8) _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 La1 O2 2.248(6) . ? La1 O1 2.268(6) . ? La1 N3 2.422(7) . ? La1 O3 2.619(7) . ? La1 N1 2.699(7) . ? La1 N2 2.721(6) . ? La1 C14 2.954(9) . ? Si1 N3 1.704(8) . ? Si1 C35 1.871(11) . ? Si1 C36 1.877(12) . ? Si1 C34 1.879(13) . ? Si2 N3 1.715(7) . ? Si2 C38 1.834(14) . ? Si2 C39 1.846(12) . ? Si2 C37 1.887(11) . ? O1 C1 1.330(10) . ? O2 C7 1.347(10) . ? O3 C43' 1.453(19) . ? O3 C40 1.454(18) . ? O3 C40' 1.466(18) . ? O3 C43 1.47(4) . ? N1 C14 1.460(10) . ? N1 C15 1.489(10) . ? N1 C13 1.491(12) . ? N2 C14 1.430(11) . ? N2 C16 1.469(11) . ? N2 C17 1.472(11) . ? C1 C6 1.402(12) . ? C1 C2 1.435(11) . ? C2 C3 1.378(12) . ? C2 C18 1.527(12) . ? C3 C4 1.394(12) . ? C3 H3 0.9300 . ? C4 C5 1.399(13) . ? C4 C22 1.506(12) . ? C5 C6 1.390(12) . ? C5 H5 0.9300 . ? C6 C13 1.500(12) . ? C7 C8 1.416(12) . ? C7 C12 1.417(12) . ? C8 C9 1.412(12) . ? C8 C26 1.531(12) . ? C9 C10 1.398(13) . ? C9 H9 0.9300 . ? C10 C11 1.388(13) . ? C10 C30 1.532(13) . ? C11 C12 1.403(12) . ? C11 H11 0.9300 . ? C12 C17 1.500(12) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.501(12) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C20 1.501(14) . ? C18 C19 1.537(12) . ? C18 C21 1.551(13) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.516(14) . ? C22 C25 1.519(14) . ? C22 C24 1.561(15) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C28 1.508(14) . ? C26 C29 1.527(14) . ? C26 C27 1.547(13) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C33 1.519(15) . ? C30 C32 1.524(16) . ? C30 C31 1.543(16) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.496(18) . ? C40' C41' 1.493(18) . ? C41 C42 1.517(19) . ? C41' C42' 1.506(19) . ? C42 C43 1.529(19) . ? C42' C43' 1.522(19) . ? 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 O2 La1 O1 109.8(2) . . ? O2 La1 N3 125.6(3) . . ? O1 La1 N3 124.4(2) . . ? O2 La1 O3 89.9(2) . . ? O1 La1 O3 90.0(2) . . ? N3 La1 O3 85.3(3) . . ? O2 La1 N1 104.7(2) . . ? O1 La1 N1 69.5(2) . . ? N3 La1 N1 99.0(2) . . ? O3 La1 N1 157.8(2) . . ? O2 La1 N2 68.8(2) . . ? O1 La1 N2 110.1(2) . . ? N3 La1 N2 95.5(2) . . ? O3 La1 N2 154.4(2) . . ? N1 La1 N2 47.4(2) . . ? O2 La1 C14 75.3(2) . . ? O1 La1 C14 81.4(2) . . ? N3 La1 C14 115.4(2) . . ? O3 La1 C14 159.0(2) . . ? N1 La1 C14 29.5(2) . . ? N2 La1 C14 28.8(2) . . ? N3 Si1 C35 115.5(5) . . ? N3 Si1 C36 110.5(5) . . ? C35 Si1 C36 104.6(6) . . ? N3 Si1 C34 114.2(6) . . ? C35 Si1 C34 106.4(6) . . ? C36 Si1 C34 104.6(7) . . ? N3 Si2 C38 110.3(5) . . ? N3 Si2 C39 114.3(5) . . ? C38 Si2 C39 105.6(8) . . ? N3 Si2 C37 114.4(6) . . ? C38 Si2 C37 104.4(7) . . ? C39 Si2 C37 107.1(6) . . ? C1 O1 La1 143.9(5) . . ? C7 O2 La1 149.1(6) . . ? C43' O3 C40 94(2) . . ? C43' O3 C40' 105.9(18) . . ? C40 O3 C40' 45.1(16) . . ? C43' O3 C43 33(2) . . ? C40 O3 C43 107.1(18) . . ? C40' O3 C43 93.8(19) . . ? C43' O3 La1 126.0(15) . . ? C40 O3 La1 134.2(11) . . ? C40' O3 La1 124.7(12) . . ? C43 O3 La1 118.6(15) . . ? C14 N1 C15 103.0(6) . . ? C14 N1 C13 116.9(7) . . ? C15 N1 C13 112.4(7) . . ? C14 N1 La1 85.0(5) . . ? C15 N1 La1 111.2(5) . . ? C13 N1 La1 123.9(5) . . ? C14 N2 C16 103.9(7) . . ? C14 N2 C17 117.3(7) . . ? C16 N2 C17 113.5(7) . . ? C14 N2 La1 84.7(5) . . ? C16 N2 La1 110.6(5) . . ? C17 N2 La1 122.5(5) . . ? Si1 N3 Si2 124.0(4) . . ? Si1 N3 La1 118.5(4) . . ? Si2 N3 La1 117.4(4) . . ? O1 C1 C6 119.8(8) . . ? O1 C1 C2 122.2(7) . . ? C6 C1 C2 117.9(8) . . ? C3 C2 C1 118.2(8) . . ? C3 C2 C18 120.9(8) . . ? C1 C2 C18 120.9(8) . . ? C2 C3 C4 125.1(9) . . ? C2 C3 H3 117.4 . . ? C4 C3 H3 117.4 . . ? C3 C4 C5 115.1(8) . . ? C3 C4 C22 121.2(8) . . ? C5 C4 C22 123.7(8) . . ? C6 C5 C4 122.8(9) . . ? C6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C5 C6 C1 120.6(9) . . ? C5 C6 C13 116.4(8) . . ? C1 C6 C13 122.5(8) . . ? O2 C7 C8 122.1(8) . . ? O2 C7 C12 118.7(8) . . ? C8 C7 C12 119.2(8) . . ? C9 C8 C7 117.7(8) . . ? C9 C8 C26 121.3(8) . . ? C7 C8 C26 120.9(8) . . ? C10 C9 C8 124.6(8) . . ? C10 C9 H9 117.7 . . ? C8 C9 H9 117.7 . . ? C11 C10 C9 115.6(8) . . ? C11 C10 C30 124.1(9) . . ? C9 C10 C30 120.1(8) . . ? C10 C11 C12 123.3(9) . . ? C10 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C7 119.5(8) . . ? C11 C12 C17 116.9(8) . . ? C7 C12 C17 123.2(8) . . ? N1 C13 C6 115.6(7) . . ? N1 C13 H13A 108.4 . . ? C6 C13 H13A 108.4 . . ? N1 C13 H13B 108.4 . . ? C6 C13 H13B 108.4 . . ? H13A C13 H13B 107.4 . . ? N2 C14 N1 97.7(6) . . ? N2 C14 La1 66.5(4) . . ? N1 C14 La1 65.5(4) . . ? N2 C14 H14A 112.2 . . ? N1 C14 H14A 112.2 . . ? La1 C14 H14A 176.9 . . ? N2 C14 H14B 112.2 . . ? N1 C14 H14B 112.2 . . ? La1 C14 H14B 73.2 . . ? H14A C14 H14B 109.8 . . ? N1 C15 C16 102.6(7) . . ? N1 C15 H15A 111.2 . . ? C16 C15 H15A 111.2 . . ? N1 C15 H15B 111.2 . . ? C16 C15 H15B 111.2 . . ? H15A C15 H15B 109.2 . . ? N2 C16 C15 103.8(7) . . ? N2 C16 H16A 111.0 . . ? C15 C16 H16A 111.0 . . ? N2 C16 H16B 111.0 . . ? C15 C16 H16B 111.0 . . ? H16A C16 H16B 109.0 . . ? N2 C17 C12 116.3(7) . . ? N2 C17 H17A 108.2 . . ? C12 C17 H17A 108.2 . . ? N2 C17 H17B 108.2 . . ? C12 C17 H17B 108.2 . . ? H17A C17 H17B 107.4 . . ? C20 C18 C2 110.9(8) . . ? C20 C18 C19 107.5(8) . . ? C2 C18 C19 112.6(8) . . ? C20 C18 C21 109.8(9) . . ? C2 C18 C21 109.9(8) . . ? C19 C18 C21 106.1(8) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C4 C22 C23 111.3(9) . . ? C4 C22 C25 113.8(8) . . ? C23 C22 C25 108.6(8) . . ? C4 C22 C24 109.0(8) . . ? C23 C22 C24 107.9(9) . . ? C25 C22 C24 106.0(9) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C28 C26 C29 112.1(9) . . ? C28 C26 C8 110.3(8) . . ? C29 C26 C8 109.6(8) . . ? C28 C26 C27 105.8(9) . . ? C29 C26 C27 107.4(9) . . ? C8 C26 C27 111.6(8) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C33 C30 C32 109.8(11) . . ? C33 C30 C10 109.7(9) . . ? C32 C30 C10 111.2(9) . . ? C33 C30 C31 109.0(10) . . ? C32 C30 C31 108.4(10) . . ? C10 C30 C31 108.8(9) . . ? 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 . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si2 C37 H37A 109.5 . . ? Si2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si2 C38 H38A 109.5 . . ? Si2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si2 C39 H39A 109.5 . . ? Si2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O3 C40 C41 106.8(19) . . ? O3 C40' C41' 112(2) . . ? C40 C41 C42 94(2) . . ? C40' C41' C42' 102(2) . . ? C41 C42 C43 100(3) . . ? C41' C42' C43' 106(3) . . ? O3 C43 C42 98(3) . . ? O3 C43' C42' 108(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.025 _refine_diff_density_min -2.351 _refine_diff_density_rms 0.141 #===================================================end data_complex2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H76 N3 O3 Pr Si2' _chemical_formula_sum 'C43 H76 N3 O3 Pr Si2' _chemical_formula_weight 880.16 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' 'Pr' 'Pr' -0.2180 2.8214 '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 10.3377(9) _cell_length_b 20.5374(18) _cell_length_c 22.632(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.196(2) _cell_angle_gamma 90.00 _cell_volume 4729.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14958 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 1.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.604 _exptl_absorpt_correction_T_max 0.800 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45766 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8647 _reflns_number_gt 7199 _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 ? _computing_publication_material ? _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^)+(0.0289P)^2^+14.2123P] 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 8647 _refine_ls_number_parameters 478 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.60579(3) 0.509375(14) 0.710316(13) 0.02684(10) Uani 1 1 d . . . Si1 Si 0.42772(18) 0.37696(9) 0.75531(9) 0.0464(5) Uani 1 1 d . . . Si2 Si 0.36652(17) 0.41031(9) 0.62347(8) 0.0421(4) Uani 1 1 d . . . O1 O 0.6334(4) 0.58345(17) 0.64043(17) 0.0343(9) Uani 1 1 d . . . O2 O 0.7203(4) 0.54144(18) 0.79848(16) 0.0335(9) Uani 1 1 d . . . O3 O 0.4106(4) 0.5782(2) 0.73115(19) 0.0473(11) Uani 1 1 d . . . N1 N 0.7802(4) 0.4645(2) 0.64665(19) 0.0262(10) Uani 1 1 d . . . N2 N 0.8166(4) 0.43455(19) 0.74132(19) 0.0254(10) Uani 1 1 d . . . N3 N 0.4524(4) 0.4212(2) 0.6948(2) 0.0340(11) Uani 1 1 d . . . C1 C 0.7227(5) 0.6092(3) 0.6117(2) 0.0302(12) Uani 1 1 d . . . C2 C 0.7227(5) 0.6769(3) 0.5975(2) 0.0282(12) Uani 1 1 d . . . C3 C 0.8266(5) 0.7007(3) 0.5727(3) 0.0350(14) Uani 1 1 d . . . H3 H 0.8285 0.7457 0.5653 0.042 Uiso 1 1 calc R . . C4 C 0.9283(5) 0.6631(3) 0.5580(2) 0.0294(12) Uani 1 1 d . . . C5 C 0.9203(5) 0.5968(3) 0.5680(2) 0.0331(13) Uani 1 1 d . . . H5 H 0.9853 0.5693 0.5574 0.040 Uiso 1 1 calc R . . C6 C 0.8188(5) 0.5690(3) 0.5935(2) 0.0305(13) Uani 1 1 d . . . C7 C 0.8367(5) 0.5423(3) 0.8357(2) 0.0289(12) Uani 1 1 d . . . C8 C 0.8727(6) 0.5956(3) 0.8760(2) 0.0304(13) Uani 1 1 d . . . C9 C 0.9962(6) 0.5942(3) 0.9124(2) 0.0356(14) Uani 1 1 d . . . H9 H 1.0198 0.6291 0.9389 0.043 Uiso 1 1 calc R . . C10 C 1.0873(5) 0.5439(3) 0.9119(3) 0.0350(14) Uani 1 1 d . . . C11 C 1.0486(5) 0.4926(3) 0.8735(2) 0.0309(12) Uani 1 1 d . . . H11 H 1.1069 0.4577 0.8722 0.037 Uiso 1 1 calc R . . C12 C 0.9251(5) 0.4909(3) 0.8364(2) 0.0276(12) Uani 1 1 d . . . C13 C 0.8085(6) 0.4956(3) 0.5917(2) 0.0314(12) Uani 1 1 d . . . H13A H 0.7391 0.4833 0.5582 0.038 Uiso 1 1 calc R . . H13B H 0.8914 0.4779 0.5833 0.038 Uiso 1 1 calc R . . C14 C 0.8771(5) 0.4760(3) 0.7017(2) 0.0281(12) Uani 1 1 d . . . H14A H 0.9654 0.4612 0.6979 0.034 Uiso 1 1 calc R . . H14B H 0.8801 0.5218 0.7142 0.034 Uiso 1 1 calc R . . C15 C 0.7767(6) 0.3926(2) 0.6433(3) 0.0346(14) Uani 1 1 d . . . H15A H 0.8455 0.3759 0.6226 0.042 Uiso 1 1 calc R . . H15B H 0.6910 0.3772 0.6224 0.042 Uiso 1 1 calc R . . C16 C 0.8010(6) 0.3721(3) 0.7085(3) 0.0342(13) Uani 1 1 d . . . H16A H 0.7263 0.3473 0.7181 0.041 Uiso 1 1 calc R . . H16B H 0.8806 0.3455 0.7181 0.041 Uiso 1 1 calc R . . C17 C 0.8889(6) 0.4276(3) 0.8030(2) 0.0329(13) Uani 1 1 d . . . H17A H 0.9698 0.4032 0.8017 0.039 Uiso 1 1 calc R . . H17B H 0.8355 0.4016 0.8259 0.039 Uiso 1 1 calc R . . C18 C 0.6093(5) 0.7210(3) 0.6062(3) 0.0314(13) Uani 1 1 d . . . C19 C 0.6223(6) 0.7899(3) 0.5817(3) 0.0439(16) Uani 1 1 d . . . H19A H 0.7024 0.8098 0.6028 0.066 Uiso 1 1 calc R . . H19B H 0.5473 0.8159 0.5876 0.066 Uiso 1 1 calc R . . H19C H 0.6255 0.7876 0.5392 0.066 Uiso 1 1 calc R . . C20 C 0.6021(7) 0.7275(3) 0.6731(3) 0.0498(17) Uani 1 1 d . . . H20A H 0.5898 0.6848 0.6895 0.075 Uiso 1 1 calc R . . H20B H 0.5289 0.7554 0.6777 0.075 Uiso 1 1 calc R . . H20C H 0.6832 0.7464 0.6942 0.075 Uiso 1 1 calc R . . C21 C 0.4809(6) 0.6929(3) 0.5715(3) 0.0423(15) Uani 1 1 d . . . H21A H 0.4853 0.6912 0.5290 0.063 Uiso 1 1 calc R . . H21B H 0.4080 0.7204 0.5775 0.063 Uiso 1 1 calc R . . H21C H 0.4680 0.6493 0.5859 0.063 Uiso 1 1 calc R . . C22 C 1.0373(6) 0.6945(3) 0.5297(3) 0.0352(14) Uani 1 1 d . . . C23 C 1.1053(7) 0.7485(3) 0.5706(3) 0.0556(19) Uani 1 1 d . . . H23A H 1.1758 0.7671 0.5529 0.083 Uiso 1 1 calc R . . H23B H 1.1412 0.7304 0.6096 0.083 Uiso 1 1 calc R . . H23C H 1.0420 0.7822 0.5751 0.083 Uiso 1 1 calc R . . C24 C 0.9781(7) 0.7237(3) 0.4691(3) 0.0540(18) Uani 1 1 d . . . H24A H 1.0474 0.7427 0.4508 0.081 Uiso 1 1 calc R . . H24B H 0.9153 0.7572 0.4747 0.081 Uiso 1 1 calc R . . H24C H 0.9340 0.6898 0.4432 0.081 Uiso 1 1 calc R . . C25 C 1.1424(6) 0.6450(3) 0.5199(3) 0.0465(16) Uani 1 1 d . . . H25A H 1.1032 0.6122 0.4915 0.070 Uiso 1 1 calc R . . H25B H 1.1786 0.6244 0.5578 0.070 Uiso 1 1 calc R . . H25C H 1.2120 0.6671 0.5041 0.070 Uiso 1 1 calc R . . C26 C 0.7754(6) 0.6503(3) 0.8816(3) 0.0373(14) Uani 1 1 d . . . C27 C 0.8317(7) 0.7006(3) 0.9294(4) 0.063(2) Uani 1 1 d . . . H27A H 0.8517 0.6795 0.9683 0.095 Uiso 1 1 calc R . . H27B H 0.7676 0.7348 0.9307 0.095 Uiso 1 1 calc R . . H27C H 0.9113 0.7192 0.9195 0.095 Uiso 1 1 calc R . . C28 C 0.6534(6) 0.6223(3) 0.9011(3) 0.0534(18) Uani 1 1 d . . . H28A H 0.6139 0.5901 0.8720 0.080 Uiso 1 1 calc R . . H28B H 0.5909 0.6570 0.9035 0.080 Uiso 1 1 calc R . . H28C H 0.6777 0.6019 0.9401 0.080 Uiso 1 1 calc R . . C29 C 0.7397(8) 0.6865(3) 0.8222(3) 0.065(2) Uani 1 1 d . . . H29A H 0.8186 0.7049 0.8112 0.097 Uiso 1 1 calc R . . H29B H 0.6783 0.7212 0.8263 0.097 Uiso 1 1 calc R . . H29C H 0.6996 0.6565 0.7912 0.097 Uiso 1 1 calc R . . C30 C 1.2193(6) 0.5458(3) 0.9554(3) 0.0428(15) Uani 1 1 d . . . C31 C 1.2916(7) 0.6098(4) 0.9490(3) 0.065(2) Uani 1 1 d . . . H31A H 1.3733 0.6106 0.9777 0.098 Uiso 1 1 calc R . . H31B H 1.2369 0.6461 0.9567 0.098 Uiso 1 1 calc R . . H31C H 1.3103 0.6132 0.9086 0.098 Uiso 1 1 calc R . . C32 C 1.3081(6) 0.4888(4) 0.9444(3) 0.066(2) Uani 1 1 d . . . H32A H 1.2651 0.4480 0.9506 0.099 Uiso 1 1 calc R . . H32B H 1.3909 0.4916 0.9721 0.099 Uiso 1 1 calc R . . H32C H 1.3243 0.4907 0.9035 0.099 Uiso 1 1 calc R . . C33 C 1.1931(7) 0.5411(4) 1.0202(3) 0.0509(17) Uani 1 1 d . . . H33A H 1.1531 0.4993 1.0260 0.076 Uiso 1 1 calc R . . H33B H 1.1343 0.5758 1.0274 0.076 Uiso 1 1 calc R . . H33C H 1.2755 0.5451 1.0482 0.076 Uiso 1 1 calc R . . C34 C 0.5259(7) 0.4119(4) 0.8258(3) 0.065(2) Uani 1 1 d . . . H34A H 0.6186 0.4107 0.8233 0.097 Uiso 1 1 calc R . . H34B H 0.5107 0.3865 0.8600 0.097 Uiso 1 1 calc R . . H34C H 0.4993 0.4566 0.8304 0.097 Uiso 1 1 calc R . . C35 C 0.4822(9) 0.2901(3) 0.7551(4) 0.079(3) Uani 1 1 d . . . H35A H 0.4303 0.2675 0.7213 0.118 Uiso 1 1 calc R . . H35B H 0.4702 0.2693 0.7922 0.118 Uiso 1 1 calc R . . H35C H 0.5743 0.2885 0.7516 0.118 Uiso 1 1 calc R . . C36 C 0.2532(7) 0.3736(5) 0.7676(4) 0.085(3) Uani 1 1 d . . . H36A H 0.2168 0.4172 0.7655 0.128 Uiso 1 1 calc R . . H36B H 0.2506 0.3551 0.8068 0.128 Uiso 1 1 calc R . . H36C H 0.2019 0.3467 0.7368 0.128 Uiso 1 1 calc R . . C37 C 0.1875(6) 0.4315(4) 0.6141(4) 0.065(2) Uani 1 1 d . . . H37A H 0.1450 0.4030 0.6390 0.098 Uiso 1 1 calc R . . H37B H 0.1467 0.4261 0.5724 0.098 Uiso 1 1 calc R . . H37C H 0.1782 0.4764 0.6262 0.098 Uiso 1 1 calc R . . C38 C 0.4320(8) 0.4645(4) 0.5694(3) 0.076(3) Uani 1 1 d . . . H38A H 0.4237 0.5096 0.5810 0.114 Uiso 1 1 calc R . . H38B H 0.3824 0.4576 0.5294 0.114 Uiso 1 1 calc R . . H38C H 0.5238 0.4544 0.5699 0.114 Uiso 1 1 calc R . . C39 C 0.3754(7) 0.3256(4) 0.5946(3) 0.066(2) Uani 1 1 d . . . H39A H 0.4668 0.3129 0.5978 0.099 Uiso 1 1 calc R . . H39B H 0.3325 0.3238 0.5529 0.099 Uiso 1 1 calc R . . H39C H 0.3317 0.2961 0.6182 0.099 Uiso 1 1 calc R . . C40 C 0.3758(17) 0.6033(10) 0.7878(9) 0.081(5) Uiso 0.50 1 d PD . . C40' C 0.3383(18) 0.5634(9) 0.7792(8) 0.077(5) Uiso 0.50 1 d P . . C41 C 0.2367(16) 0.6283(9) 0.7704(7) 0.072(4) Uiso 0.50 1 d PD . . C41' C 0.2046(18) 0.5935(9) 0.7676(7) 0.072(4) Uiso 0.50 1 d PD . . C42 C 0.1871(16) 0.5951(9) 0.7106(8) 0.078(4) Uiso 0.50 1 d PD . . C42' C 0.1917(16) 0.6255(9) 0.7076(7) 0.078(4) Uiso 0.50 1 d PD . . C43 C 0.3125(10) 0.6045(5) 0.6834(5) 0.098(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.02347(17) 0.03020(18) 0.02672(17) 0.00051(13) 0.00407(12) -0.00040(13) Si1 0.0385(10) 0.0495(11) 0.0536(12) 0.0025(9) 0.0147(9) -0.0098(8) Si2 0.0286(9) 0.0478(11) 0.0476(11) -0.0085(8) 0.0003(8) -0.0031(7) O1 0.036(2) 0.032(2) 0.038(2) 0.0101(17) 0.0135(19) 0.0060(17) O2 0.033(2) 0.036(2) 0.030(2) -0.0018(16) -0.0007(18) 0.0070(17) O3 0.040(3) 0.062(3) 0.040(3) 0.007(2) 0.007(2) 0.018(2) N1 0.026(2) 0.026(2) 0.026(2) -0.0021(18) 0.0053(19) -0.0019(18) N2 0.030(3) 0.019(2) 0.027(2) -0.0025(18) 0.005(2) -0.0008(18) N3 0.028(3) 0.036(3) 0.037(3) -0.005(2) 0.006(2) -0.007(2) C1 0.027(3) 0.033(3) 0.031(3) 0.004(2) 0.008(2) 0.001(2) C2 0.029(3) 0.037(3) 0.019(3) 0.001(2) 0.006(2) 0.002(2) C3 0.032(3) 0.033(3) 0.039(4) 0.000(2) 0.003(3) -0.001(2) C4 0.026(3) 0.033(3) 0.028(3) 0.001(2) 0.002(2) -0.005(2) C5 0.030(3) 0.042(4) 0.027(3) 0.001(2) 0.005(3) 0.003(3) C6 0.028(3) 0.032(3) 0.030(3) 0.005(2) 0.003(2) 0.000(2) C7 0.026(3) 0.032(3) 0.028(3) 0.002(2) 0.003(2) -0.003(2) C8 0.039(3) 0.028(3) 0.024(3) -0.001(2) 0.006(3) 0.000(2) C9 0.038(3) 0.041(4) 0.027(3) -0.006(2) 0.002(3) -0.007(3) C10 0.026(3) 0.050(4) 0.029(3) 0.001(3) 0.004(3) -0.006(3) C11 0.030(3) 0.038(3) 0.024(3) -0.001(2) 0.003(2) 0.003(2) C12 0.027(3) 0.031(3) 0.024(3) -0.002(2) 0.003(2) -0.002(2) C13 0.034(3) 0.031(3) 0.030(3) 0.001(2) 0.008(2) 0.005(2) C14 0.028(3) 0.028(3) 0.028(3) -0.003(2) 0.003(2) 0.000(2) C15 0.044(4) 0.020(3) 0.041(4) -0.009(2) 0.011(3) -0.004(2) C16 0.035(3) 0.031(3) 0.036(3) 0.000(2) 0.006(3) -0.002(2) C17 0.034(3) 0.033(3) 0.030(3) 0.004(2) 0.002(3) 0.007(2) C18 0.030(3) 0.029(3) 0.036(3) 0.003(2) 0.008(3) 0.001(2) C19 0.049(4) 0.035(4) 0.048(4) 0.008(3) 0.010(3) 0.005(3) C20 0.067(5) 0.051(4) 0.035(4) 0.000(3) 0.017(3) 0.013(3) C21 0.032(3) 0.046(4) 0.048(4) 0.006(3) 0.006(3) 0.008(3) C22 0.028(3) 0.035(3) 0.043(4) 0.000(3) 0.005(3) -0.006(2) C23 0.042(4) 0.050(4) 0.079(5) -0.018(4) 0.020(4) -0.013(3) C24 0.041(4) 0.068(5) 0.057(5) 0.018(4) 0.020(3) -0.009(3) C25 0.040(4) 0.050(4) 0.053(4) -0.006(3) 0.020(3) -0.004(3) C26 0.045(4) 0.027(3) 0.039(4) -0.006(2) 0.005(3) 0.001(3) C27 0.052(5) 0.048(4) 0.087(6) -0.030(4) 0.003(4) -0.003(3) C28 0.046(4) 0.045(4) 0.070(5) -0.013(3) 0.014(4) 0.006(3) C29 0.092(6) 0.045(4) 0.055(5) 0.012(3) 0.009(4) 0.014(4) C30 0.033(3) 0.062(4) 0.031(3) -0.002(3) -0.001(3) -0.005(3) C31 0.043(4) 0.092(6) 0.059(5) 0.001(4) 0.004(4) -0.026(4) C32 0.032(4) 0.102(6) 0.058(5) -0.025(4) -0.010(3) 0.009(4) C33 0.050(4) 0.070(5) 0.030(4) -0.007(3) 0.000(3) -0.008(3) C34 0.059(5) 0.090(6) 0.044(4) 0.001(4) 0.006(4) -0.007(4) C35 0.099(7) 0.049(5) 0.092(7) 0.014(4) 0.029(5) -0.017(4) C36 0.042(5) 0.138(8) 0.082(6) 0.014(6) 0.030(5) -0.020(5) C37 0.038(4) 0.070(5) 0.083(6) -0.025(4) -0.002(4) 0.003(3) C38 0.061(5) 0.111(7) 0.051(5) 0.018(5) -0.006(4) -0.017(5) C39 0.056(5) 0.070(5) 0.066(5) -0.026(4) -0.004(4) 0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O2 2.232(4) . ? Pr1 O1 2.249(4) . ? Pr1 N3 2.391(4) . ? Pr1 O3 2.575(4) . ? Pr1 N2 2.657(4) . ? Pr1 N1 2.664(4) . ? Pr1 C14 2.927(5) . ? Si1 N3 1.701(5) . ? Si1 C35 1.871(8) . ? Si1 C36 1.875(7) . ? Si1 C34 1.875(7) . ? Si2 N3 1.713(5) . ? Si2 C39 1.866(7) . ? Si2 C38 1.867(8) . ? Si2 C37 1.877(7) . ? O1 C1 1.329(6) . ? O2 C7 1.340(6) . ? O3 C43 1.449(11) . ? O3 C40' 1.456(19) . ? O3 C40 1.485(19) . ? N1 C13 1.472(7) . ? N1 C14 1.474(6) . ? N1 C15 1.478(7) . ? N2 C14 1.456(6) . ? N2 C17 1.469(7) . ? N2 C16 1.477(7) . ? C1 C6 1.410(8) . ? C1 C2 1.425(8) . ? C2 C3 1.386(8) . ? C2 C18 1.522(7) . ? C3 C4 1.392(8) . ? C3 H3 0.9400 . ? C4 C5 1.386(8) . ? C4 C22 1.534(8) . ? C5 C6 1.405(8) . ? C5 H5 0.9400 . ? C6 C13 1.511(7) . ? C7 C12 1.395(7) . ? C7 C8 1.431(7) . ? C8 C9 1.391(8) . ? C8 C26 1.528(8) . ? C9 C10 1.399(8) . ? C9 H9 0.9400 . ? C10 C11 1.379(8) . ? C10 C30 1.536(8) . ? C11 C12 1.398(7) . ? C11 H11 0.9400 . ? C12 C17 1.518(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.513(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 C21 1.530(8) . ? C18 C20 1.534(8) . ? C18 C19 1.535(8) . ? 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 C24 1.522(8) . ? C22 C25 1.532(8) . ? C22 C23 1.533(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 C28 1.520(9) . ? C26 C29 1.524(9) . ? C26 C27 1.534(8) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 C31 1.531(9) . ? C30 C32 1.535(9) . ? C30 C33 1.541(8) . ? 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 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? 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 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C40 C41 1.512(16) . ? C40' C41' 1.49(2) . ? C41 C42 1.520(16) . ? C41' C42' 1.493(16) . ? C42 C43 1.542(15) . ? C42' C43 1.514(15) . ? 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 O2 Pr1 O1 108.41(14) . . ? O2 Pr1 N3 126.02(15) . . ? O1 Pr1 N3 124.89(15) . . ? O2 Pr1 O3 89.05(13) . . ? O1 Pr1 O3 87.63(13) . . ? N3 Pr1 O3 85.51(15) . . ? O2 Pr1 N2 69.75(13) . . ? O1 Pr1 N2 112.13(13) . . ? N3 Pr1 N2 95.31(14) . . ? O3 Pr1 N2 154.39(13) . . ? O2 Pr1 N1 106.43(13) . . ? O1 Pr1 N1 70.83(13) . . ? N3 Pr1 N1 98.79(14) . . ? O3 Pr1 N1 156.43(13) . . ? N2 Pr1 N1 48.76(13) . . ? O2 Pr1 C14 76.43(14) . . ? O1 Pr1 C14 82.48(14) . . ? N3 Pr1 C14 115.55(15) . . ? O3 Pr1 C14 158.75(15) . . ? N2 Pr1 C14 29.72(13) . . ? N1 Pr1 C14 30.10(13) . . ? N3 Si1 C35 114.8(3) . . ? N3 Si1 C36 115.1(3) . . ? C35 Si1 C36 105.3(4) . . ? N3 Si1 C34 110.2(3) . . ? C35 Si1 C34 104.4(4) . . ? C36 Si1 C34 106.2(4) . . ? N3 Si2 C39 113.7(3) . . ? N3 Si2 C38 110.6(3) . . ? C39 Si2 C38 106.3(4) . . ? N3 Si2 C37 114.3(3) . . ? C39 Si2 C37 106.6(3) . . ? C38 Si2 C37 104.6(4) . . ? C1 O1 Pr1 143.0(3) . . ? C7 O2 Pr1 147.2(3) . . ? C43 O3 C40' 104.5(9) . . ? C43 O3 C40 105.7(8) . . ? C40' O3 C40 36.2(9) . . ? C43 O3 Pr1 122.4(5) . . ? C40' O3 Pr1 123.0(8) . . ? C40 O3 Pr1 131.8(7) . . ? C13 N1 C14 115.9(4) . . ? C13 N1 C15 113.4(4) . . ? C14 N1 C15 102.2(4) . . ? C13 N1 Pr1 124.1(3) . . ? C14 N1 Pr1 84.9(3) . . ? C15 N1 Pr1 111.1(3) . . ? C14 N2 C17 116.1(4) . . ? C14 N2 C16 102.7(4) . . ? C17 N2 C16 112.6(4) . . ? C14 N2 Pr1 85.4(3) . . ? C17 N2 Pr1 124.3(3) . . ? C16 N2 Pr1 111.0(3) . . ? Si1 N3 Si2 124.2(3) . . ? Si1 N3 Pr1 118.4(2) . . ? Si2 N3 Pr1 117.2(2) . . ? O1 C1 C6 119.7(5) . . ? O1 C1 C2 121.8(5) . . ? C6 C1 C2 118.5(5) . . ? C3 C2 C1 117.8(5) . . ? C3 C2 C18 120.8(5) . . ? C1 C2 C18 121.3(5) . . ? C2 C3 C4 125.0(5) . . ? C2 C3 H3 117.5 . . ? C4 C3 H3 117.5 . . ? C5 C4 C3 115.9(5) . . ? C5 C4 C22 123.5(5) . . ? C3 C4 C22 120.6(5) . . ? C4 C5 C6 122.5(5) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 119.9(5) . . ? C5 C6 C13 116.7(5) . . ? C1 C6 C13 122.9(5) . . ? O2 C7 C12 120.7(5) . . ? O2 C7 C8 121.0(5) . . ? C12 C7 C8 118.4(5) . . ? C9 C8 C7 118.0(5) . . ? C9 C8 C26 121.0(5) . . ? C7 C8 C26 120.9(5) . . ? C8 C9 C10 124.0(5) . . ? C8 C9 H9 118.0 . . ? C10 C9 H9 118.0 . . ? C11 C10 C9 116.6(5) . . ? C11 C10 C30 123.3(5) . . ? C9 C10 C30 119.9(5) . . ? C10 C11 C12 122.0(5) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C7 C12 C11 121.0(5) . . ? C7 C12 C17 122.6(5) . . ? C11 C12 C17 116.0(5) . . ? N1 C13 C6 115.8(4) . . ? N1 C13 H13A 108.3 . . ? C6 C13 H13A 108.3 . . ? N1 C13 H13B 108.3 . . ? C6 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? N2 C14 N1 97.2(4) . . ? N2 C14 Pr1 64.8(3) . . ? N1 C14 Pr1 65.0(2) . . ? N2 C14 H14A 112.3 . . ? N1 C14 H14A 112.3 . . ? Pr1 C14 H14A 175.2 . . ? N2 C14 H14B 112.3 . . ? N1 C14 H14B 112.3 . . ? Pr1 C14 H14B 74.9 . . ? H14A C14 H14B 109.9 . . ? N1 C15 C16 103.3(4) . . ? N1 C15 H15A 111.1 . . ? C16 C15 H15A 111.1 . . ? N1 C15 H15B 111.1 . . ? C16 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? N2 C16 C15 103.5(4) . . ? N2 C16 H16A 111.1 . . ? C15 C16 H16A 111.1 . . ? N2 C16 H16B 111.1 . . ? C15 C16 H16B 111.1 . . ? H16A C16 H16B 109.0 . . ? N2 C17 C12 115.4(4) . . ? N2 C17 H17A 108.4 . . ? C12 C17 H17A 108.4 . . ? N2 C17 H17B 108.4 . . ? C12 C17 H17B 108.4 . . ? H17A C17 H17B 107.5 . . ? C2 C18 C21 109.1(5) . . ? C2 C18 C20 110.6(5) . . ? C21 C18 C20 110.5(5) . . ? C2 C18 C19 112.5(5) . . ? C21 C18 C19 106.6(5) . . ? C20 C18 C19 107.4(5) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C25 108.2(5) . . ? C24 C22 C23 109.1(5) . . ? C25 C22 C23 107.8(5) . . ? C24 C22 C4 109.5(5) . . ? C25 C22 C4 111.9(5) . . ? C23 C22 C4 110.1(5) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C28 C26 C29 110.9(6) . . ? C28 C26 C8 109.8(5) . . ? C29 C26 C8 110.2(5) . . ? C28 C26 C27 106.3(5) . . ? C29 C26 C27 107.3(6) . . ? C8 C26 C27 112.4(5) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C32 108.9(6) . . ? C31 C30 C10 110.7(5) . . ? C32 C30 C10 111.4(5) . . ? C31 C30 C33 108.4(5) . . ? C32 C30 C33 108.5(6) . . ? C10 C30 C33 108.9(5) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? 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 . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si2 C37 H37A 109.5 . . ? Si2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si2 C38 H38A 109.5 . . ? Si2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si2 C39 H39A 109.5 . . ? Si2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O3 C40 C41 104.9(13) . . ? O3 C40' C41' 111.3(14) . . ? C40 C41 C42 103.7(14) . . ? C42' C41' C40' 105.8(14) . . ? C41 C42 C43 97.1(12) . . ? C41' C42' C43 104.9(13) . . ? O3 C43 C42' 110.5(9) . . ? O3 C43 C42 100.5(9) . . ? C42' C43 C42 23.8(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.352 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.104 #===================================================end data_complex3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H76 N3 Nd O3 Si2, C7 H8' _chemical_formula_sum 'C50 H84 N3 Nd O3 Si2' _chemical_formula_weight 975.62 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/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 14.9057(18) _cell_length_b 32.608(3) _cell_length_c 12.3209(15) _cell_angle_alpha 90.00 _cell_angle_beta 112.249(3) _cell_angle_gamma 90.00 _cell_volume 5542.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 18533 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description 'block' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2068 _exptl_absorpt_coefficient_mu 1.018 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.683 _exptl_absorpt_correction_T_max 0.816 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51669 _diffrn_reflns_av_R_equivalents 0.0840 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.35 _reflns_number_total 10110 _reflns_number_gt 7848 _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 ? _computing_publication_material ? _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^)+(0.0477P)^2^+20.0438P] 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 10110 _refine_ls_number_parameters 520 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1170 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.1743 _refine_ls_wR_factor_gt 0.1625 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 1.10034(3) 0.137596(12) 0.30409(3) 0.04288(15) Uani 1 1 d . . . Si1 Si 1.31795(18) 0.13895(9) 0.5540(3) 0.0759(8) Uani 1 1 d . . . Si2 Si 1.3133(2) 0.19383(9) 0.3576(3) 0.0805(8) Uani 1 1 d . . . O1 O 1.0201(4) 0.16053(15) 0.1228(4) 0.0520(13) Uani 1 1 d . . . O2 O 1.0252(4) 0.08383(16) 0.3436(4) 0.0541(13) Uani 1 1 d . . . O3 O 1.1832(4) 0.08528(18) 0.2197(5) 0.0704(16) Uani 1 1 d D . . N1 N 1.0167(4) 0.20753(17) 0.3145(5) 0.0419(14) Uani 1 1 d . . . N2 N 1.0129(4) 0.16167(17) 0.4425(5) 0.0414(14) Uani 1 1 d . . . N3 N 1.2588(4) 0.1602(2) 0.4189(6) 0.0586(17) Uani 1 1 d . . . C1 C 0.9457(5) 0.1835(2) 0.0537(6) 0.0437(17) Uani 1 1 d . . . C2 C 0.8932(6) 0.1729(2) -0.0652(6) 0.0491(19) Uani 1 1 d . . . C3 C 0.8124(6) 0.1968(2) -0.1293(6) 0.053(2) Uani 1 1 d . . . H3 H 0.7777 0.1897 -0.2071 0.063 Uiso 1 1 calc R . . C4 C 0.7806(5) 0.2303(2) -0.0840(7) 0.0496(19) Uani 1 1 d . . . C5 C 0.8365(5) 0.2407(2) 0.0307(6) 0.0476(18) Uani 1 1 d . . . H5 H 0.8184 0.2633 0.0639 0.057 Uiso 1 1 calc R . . C6 C 0.9179(5) 0.2189(2) 0.0977(6) 0.0451(17) Uani 1 1 d . . . C7 C 0.9436(6) 0.0739(2) 0.3598(6) 0.0480(18) Uani 1 1 d . . . C8 C 0.8920(6) 0.0373(2) 0.3135(7) 0.0498(19) Uani 1 1 d . . . C9 C 0.8034(6) 0.0314(2) 0.3247(7) 0.055(2) Uani 1 1 d . . . H9 H 0.7684 0.0080 0.2914 0.066 Uiso 1 1 calc R . . C10 C 0.7637(6) 0.0580(2) 0.3819(7) 0.0520(19) Uani 1 1 d . . . C11 C 0.8196(6) 0.0921(2) 0.4325(7) 0.0531(19) Uani 1 1 d . . . H11 H 0.7958 0.1107 0.4724 0.064 Uiso 1 1 calc R . . C12 C 0.9085(5) 0.0999(2) 0.4268(6) 0.0458(18) Uani 1 1 d . . . C13 C 0.9773(6) 0.2371(2) 0.2174(6) 0.0514(19) Uani 1 1 d . . . H13A H 1.0310 0.2523 0.2108 0.062 Uiso 1 1 calc R . . H13B H 0.9369 0.2566 0.2376 0.062 Uiso 1 1 calc R . . C14 C 0.9463(5) 0.1825(2) 0.3389(6) 0.0455(18) Uani 1 1 d . . . H14A H 0.9134 0.1636 0.2756 0.055 Uiso 1 1 calc R . . H14B H 0.8990 0.1989 0.3560 0.055 Uiso 1 1 calc R . . C15 C 1.0686(6) 0.2285(2) 0.4287(6) 0.053(2) Uani 1 1 d . . . H15A H 1.0353 0.2533 0.4353 0.064 Uiso 1 1 calc R . . H15B H 1.1347 0.2352 0.4387 0.064 Uiso 1 1 calc R . . C16 C 1.0662(6) 0.1963(2) 0.5178(6) 0.053(2) Uani 1 1 d . . . H16A H 1.1312 0.1881 0.5685 0.063 Uiso 1 1 calc R . . H16B H 1.0322 0.2064 0.5657 0.063 Uiso 1 1 calc R . . C17 C 0.9688(6) 0.1334(2) 0.5006(6) 0.0499(18) Uani 1 1 d . . . H17A H 0.9288 0.1493 0.5315 0.060 Uiso 1 1 calc R . . H17B H 1.0203 0.1211 0.5668 0.060 Uiso 1 1 calc R . . C18 C 0.9254(7) 0.1376(2) -0.1251(7) 0.060(2) Uani 1 1 d . . . C19 C 0.8586(8) 0.1323(3) -0.2545(7) 0.094(4) Uani 1 1 d . . . H19A H 0.7946 0.1252 -0.2598 0.141 Uiso 1 1 calc R . . H19B H 0.8833 0.1108 -0.2887 0.141 Uiso 1 1 calc R . . H19C H 0.8563 0.1574 -0.2960 0.141 Uiso 1 1 calc R . . C20 C 0.9230(8) 0.0970(2) -0.0627(8) 0.078(3) Uani 1 1 d . . . H20A H 0.9615 0.0996 0.0195 0.116 Uiso 1 1 calc R . . H20B H 0.9488 0.0755 -0.0954 0.116 Uiso 1 1 calc R . . H20C H 0.8573 0.0907 -0.0733 0.116 Uiso 1 1 calc R . . C21 C 1.0267(7) 0.1471(3) -0.1211(8) 0.077(3) Uani 1 1 d . . . H21A H 1.0242 0.1708 -0.1685 0.116 Uiso 1 1 calc R . . H21B H 1.0506 0.1241 -0.1506 0.116 Uiso 1 1 calc R . . H21C H 1.0693 0.1525 -0.0416 0.116 Uiso 1 1 calc R . . C22 C 0.6852(6) 0.2520(3) -0.1562(8) 0.061(2) Uani 1 1 d . . . C23 C 0.6028(7) 0.2285(4) -0.1414(11) 0.111(4) Uani 1 1 d . . . H23A H 0.6089 0.2301 -0.0611 0.166 Uiso 1 1 calc R . . H23B H 0.6052 0.2003 -0.1627 0.166 Uiso 1 1 calc R . . H23C H 0.5420 0.2403 -0.1910 0.166 Uiso 1 1 calc R . . C24 C 0.6707(8) 0.2540(4) -0.2850(9) 0.120(5) Uani 1 1 d . . . H24A H 0.6121 0.2688 -0.3275 0.180 Uiso 1 1 calc R . . H24B H 0.6660 0.2267 -0.3159 0.180 Uiso 1 1 calc R . . H24C H 0.7247 0.2679 -0.2928 0.180 Uiso 1 1 calc R . . C25 C 0.6831(7) 0.2954(3) -0.1141(10) 0.093(3) Uani 1 1 d . . . H25A H 0.7396 0.3099 -0.1129 0.139 Uiso 1 1 calc R . . H25B H 0.6823 0.2949 -0.0366 0.139 Uiso 1 1 calc R . . H25C H 0.6260 0.3091 -0.1663 0.139 Uiso 1 1 calc R . . C26 C 0.9337(7) 0.0043(2) 0.2572(7) 0.058(2) Uani 1 1 d . . . C27 C 0.8678(8) -0.0335(3) 0.2194(10) 0.091(3) Uani 1 1 d . . . H27A H 0.8608 -0.0455 0.2869 0.137 Uiso 1 1 calc R . . H27B H 0.8961 -0.0531 0.1838 0.137 Uiso 1 1 calc R . . H27C H 0.8053 -0.0254 0.1640 0.137 Uiso 1 1 calc R . . C28 C 1.0303(7) -0.0099(3) 0.3463(8) 0.077(3) Uani 1 1 d . . . H28A H 1.0695 0.0135 0.3818 0.115 Uiso 1 1 calc R . . H28B H 1.0629 -0.0263 0.3078 0.115 Uiso 1 1 calc R . . H28C H 1.0196 -0.0260 0.4056 0.115 Uiso 1 1 calc R . . C29 C 0.9452(8) 0.0212(3) 0.1472(7) 0.072(3) Uani 1 1 d . . . H29A H 0.8861 0.0343 0.0982 0.109 Uiso 1 1 calc R . . H29B H 0.9596 -0.0009 0.1050 0.109 Uiso 1 1 calc R . . H29C H 0.9972 0.0408 0.1696 0.109 Uiso 1 1 calc R . . C30 C 0.6641(6) 0.0507(3) 0.3912(8) 0.071(3) Uani 1 1 d D . . C31 C 0.5979(16) 0.0243(7) 0.2862(18) 0.103(5) Uiso 0.50 1 d PD . . C31' C 0.6290(18) 0.0071(6) 0.367(2) 0.103(5) Uiso 0.50 1 d PD . . C32 C 0.6124(17) 0.0908(6) 0.393(2) 0.098(7) Uiso 0.50 1 d PD . . C32' C 0.5936(16) 0.0840(7) 0.321(2) 0.098(7) Uiso 0.50 1 d PD . . C33 C 0.6819(17) 0.0254(7) 0.5011(17) 0.100(7) Uiso 0.50 1 d PD . . C33' C 0.6736(18) 0.0560(8) 0.5193(16) 0.106(8) Uiso 0.50 1 d PD . . C34 C 1.2388(7) 0.1002(3) 0.5857(9) 0.090(3) Uani 1 1 d . . . H34A H 1.1841 0.1138 0.5929 0.135 Uiso 1 1 calc R . . H34B H 1.2751 0.0863 0.6577 0.135 Uiso 1 1 calc R . . H34C H 1.2165 0.0807 0.5229 0.135 Uiso 1 1 calc R . . C35 C 1.3498(9) 0.1770(4) 0.6776(10) 0.128(5) Uani 1 1 d . . . H35A H 1.3841 0.1996 0.6616 0.192 Uiso 1 1 calc R . . H35B H 1.3901 0.1640 0.7494 0.192 Uiso 1 1 calc R . . H35C H 1.2916 0.1867 0.6847 0.192 Uiso 1 1 calc R . . C36 C 1.4321(8) 0.1118(5) 0.5741(13) 0.150(6) Uani 1 1 d . . . H36A H 1.4206 0.0924 0.5118 0.225 Uiso 1 1 calc R . . H36B H 1.4547 0.0976 0.6480 0.225 Uiso 1 1 calc R . . H36C H 1.4800 0.1313 0.5731 0.225 Uiso 1 1 calc R . . C37 C 1.2257(8) 0.2124(4) 0.2132(10) 0.117(4) Uani 1 1 d . . . H37A H 1.2052 0.1898 0.1594 0.175 Uiso 1 1 calc R . . H37B H 1.2564 0.2327 0.1825 0.175 Uiso 1 1 calc R . . H37C H 1.1704 0.2243 0.2232 0.175 Uiso 1 1 calc R . . C38 C 1.4163(10) 0.1715(5) 0.3260(16) 0.173(8) Uani 1 1 d . . . H38A H 1.4713 0.1682 0.3980 0.259 Uiso 1 1 calc R . . H38B H 1.4329 0.1896 0.2750 0.259 Uiso 1 1 calc R . . H38C H 1.3976 0.1453 0.2886 0.259 Uiso 1 1 calc R . . C39 C 1.3615(12) 0.2409(4) 0.4464(13) 0.164(7) Uani 1 1 d . . . H39A H 1.3087 0.2587 0.4409 0.246 Uiso 1 1 calc R . . H39B H 1.4046 0.2548 0.4172 0.246 Uiso 1 1 calc R . . H39C H 1.3962 0.2333 0.5269 0.246 Uiso 1 1 calc R . . C40 C 1.2088(18) 0.0443(6) 0.271(2) 0.095(7) Uiso 0.50 1 d PD . . C40' C 1.2531(15) 0.0584(6) 0.3095(16) 0.082(6) Uiso 0.50 1 d PD . . C41 C 1.251(2) 0.0229(7) 0.193(2) 0.111(8) Uiso 0.50 1 d PD . . C41' C 1.2997(17) 0.0321(7) 0.2452(18) 0.089(7) Uiso 0.50 1 d PD . . C42 C 1.2967(18) 0.0581(7) 0.147(2) 0.104(9) Uiso 0.50 1 d PD . . C42' C 1.257(2) 0.0448(8) 0.1176(19) 0.106(9) Uiso 0.50 1 d PD . . C43 C 1.2225(15) 0.0921(6) 0.1287(16) 0.078(6) Uiso 0.50 1 d PD . . C43' C 1.1792(16) 0.0763(7) 0.1017(15) 0.088(7) Uiso 0.50 1 d PD . . C44 C 0.646(2) 0.1043(11) 1.023(4) 0.175(4) Uiso 0.50 1 d PD . . C44' C 0.609(2) 0.1155(12) 1.037(4) 0.175(4) Uiso 0.50 1 d PD . . C45 C 0.645(2) 0.0637(11) 0.989(3) 0.175(4) Uiso 0.50 1 d PD . . C45' C 0.577(2) 0.0804(10) 0.967(3) 0.175(4) Uiso 0.50 1 d PD . . C46 C 0.552(3) 0.0438(10) 0.940(3) 0.175(4) Uiso 0.50 1 d PD . . C46' C 0.476(3) 0.0720(11) 0.916(4) 0.175(4) Uiso 0.50 1 d PD . . C47 C 0.462(3) 0.0607(11) 0.935(4) 0.175(4) Uiso 0.50 1 d PD . . C47' C 0.407(2) 0.0946(11) 0.944(3) 0.175(4) Uiso 0.50 1 d PD . . C48 C 0.467(2) 0.1030(11) 0.967(4) 0.175(4) Uiso 0.50 1 d PD . . C48' C 0.435(2) 0.1325(10) 0.998(3) 0.175(4) Uiso 0.50 1 d PD . . C49 C 0.556(3) 0.1232(12) 1.014(4) 0.175(4) Uiso 0.50 1 d PD . . C49' C 0.532(2) 0.1421(10) 1.039(4) 0.175(4) Uiso 0.50 1 d PD . . C50 C 0.745(2) 0.1218(13) 1.096(4) 0.175(4) Uiso 0.50 1 d PD . . C50' C 0.710(2) 0.1331(13) 1.087(4) 0.175(4) Uiso 0.50 1 d PD . . 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 0.0427(2) 0.0413(2) 0.0476(2) 0.0006(2) 0.02049(18) 0.0037(2) Si1 0.0509(14) 0.0773(18) 0.0875(19) 0.0061(16) 0.0128(13) 0.0020(14) Si2 0.0571(16) 0.081(2) 0.108(2) 0.0036(17) 0.0365(16) -0.0163(14) O1 0.058(3) 0.048(3) 0.048(3) -0.003(3) 0.018(3) 0.015(3) O2 0.060(3) 0.049(3) 0.061(3) -0.008(3) 0.033(3) -0.003(3) O3 0.076(4) 0.068(4) 0.076(4) 0.001(3) 0.039(3) 0.020(3) N1 0.040(3) 0.041(3) 0.044(3) -0.005(3) 0.015(3) -0.001(3) N2 0.051(4) 0.036(3) 0.040(3) 0.000(3) 0.021(3) -0.001(3) N3 0.039(4) 0.061(4) 0.076(5) 0.000(4) 0.022(3) -0.001(3) C1 0.040(4) 0.045(4) 0.047(4) 0.000(4) 0.019(3) 0.000(3) C2 0.064(5) 0.041(4) 0.042(4) 0.002(3) 0.020(4) -0.006(4) C3 0.059(5) 0.054(5) 0.041(4) 0.001(4) 0.015(4) -0.005(4) C4 0.045(4) 0.054(5) 0.052(5) 0.001(4) 0.020(4) -0.005(4) C5 0.049(4) 0.043(4) 0.055(5) 0.001(4) 0.024(4) 0.005(4) C6 0.050(5) 0.044(4) 0.046(4) 0.000(3) 0.024(4) -0.001(4) C7 0.059(5) 0.037(4) 0.053(5) 0.004(4) 0.028(4) 0.006(4) C8 0.068(5) 0.033(4) 0.053(5) 0.006(3) 0.028(4) 0.004(4) C9 0.066(5) 0.042(4) 0.057(5) -0.005(4) 0.023(4) -0.008(4) C10 0.051(5) 0.046(5) 0.064(5) 0.007(4) 0.027(4) 0.004(4) C11 0.058(5) 0.044(4) 0.060(5) 0.001(4) 0.026(4) 0.007(4) C12 0.053(5) 0.036(4) 0.052(4) 0.004(3) 0.024(4) -0.003(3) C13 0.063(5) 0.037(4) 0.055(5) 0.000(4) 0.023(4) 0.000(4) C14 0.045(4) 0.043(4) 0.048(4) -0.006(3) 0.016(4) 0.003(3) C15 0.065(5) 0.041(4) 0.049(4) -0.011(4) 0.018(4) -0.004(4) C16 0.065(5) 0.045(4) 0.046(4) -0.014(4) 0.019(4) -0.008(4) C17 0.060(5) 0.048(4) 0.046(4) -0.003(4) 0.025(4) -0.003(4) C18 0.090(6) 0.046(5) 0.049(5) 0.001(4) 0.033(4) 0.007(5) C19 0.139(10) 0.087(7) 0.047(5) -0.009(5) 0.025(6) 0.023(7) C20 0.128(9) 0.043(5) 0.065(6) -0.002(4) 0.041(6) 0.005(5) C21 0.115(8) 0.060(6) 0.078(6) 0.001(5) 0.062(6) 0.027(5) C22 0.043(5) 0.068(6) 0.070(6) 0.009(5) 0.021(4) 0.005(4) C23 0.058(6) 0.111(9) 0.156(11) 0.017(8) 0.031(7) -0.004(6) C24 0.102(9) 0.173(13) 0.073(7) 0.040(8) 0.019(6) 0.080(9) C25 0.055(6) 0.083(7) 0.121(9) 0.012(7) 0.012(6) 0.020(5) C26 0.082(6) 0.038(4) 0.066(5) -0.006(4) 0.041(5) 0.000(4) C27 0.127(9) 0.053(6) 0.116(9) -0.023(6) 0.072(8) -0.014(6) C28 0.100(8) 0.055(6) 0.093(7) 0.013(5) 0.056(6) 0.025(5) C29 0.116(8) 0.048(5) 0.065(6) -0.005(4) 0.047(6) 0.004(5) C30 0.057(5) 0.063(6) 0.098(7) 0.003(5) 0.035(5) -0.002(5) C34 0.082(7) 0.091(8) 0.086(7) 0.022(6) 0.019(6) -0.004(6) C35 0.124(10) 0.122(11) 0.095(9) -0.010(8) -0.008(8) -0.027(9) C36 0.069(8) 0.189(15) 0.186(15) 0.055(12) 0.043(9) 0.047(9) C37 0.092(8) 0.140(11) 0.122(10) 0.045(9) 0.044(8) -0.014(8) C38 0.099(10) 0.188(16) 0.27(2) 0.087(15) 0.118(13) 0.031(10) C39 0.218(17) 0.121(12) 0.153(13) -0.026(10) 0.069(13) -0.098(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O1 2.226(5) . ? Nd1 O2 2.232(5) . ? Nd1 N3 2.365(6) . ? Nd1 O3 2.548(5) . ? Nd1 N1 2.626(6) . ? Nd1 N2 2.628(5) . ? Nd1 C14 2.889(7) . ? Si1 N3 1.708(7) . ? Si1 C36 1.849(11) . ? Si1 C34 1.867(10) . ? Si1 C35 1.880(12) . ? Si2 N3 1.702(7) . ? Si2 C39 1.863(12) . ? Si2 C37 1.865(11) . ? Si2 C38 1.868(13) . ? O1 C1 1.343(8) . ? O2 C7 1.343(9) . ? O3 C43' 1.462(15) . ? O3 C43 1.464(15) . ? O3 C40 1.467(16) . ? O3 C40' 1.485(15) . ? N1 C14 1.447(9) . ? N1 C13 1.475(9) . ? N1 C15 1.491(9) . ? N2 C14 1.455(9) . ? N2 C17 1.466(9) . ? N2 C16 1.485(9) . ? C1 C6 1.401(10) . ? C1 C2 1.418(10) . ? C2 C3 1.400(10) . ? C2 C18 1.538(11) . ? C3 C4 1.390(10) . ? C3 H3 0.9300 . ? C4 C5 1.383(10) . ? C4 C22 1.534(11) . ? C5 C6 1.379(10) . ? C5 H5 0.9300 . ? C6 C13 1.524(10) . ? C7 C12 1.415(10) . ? C7 C8 1.417(10) . ? C8 C9 1.392(11) . ? C8 C26 1.535(10) . ? C9 C10 1.382(11) . ? C9 H9 0.9300 . ? C10 C11 1.388(10) . ? C10 C30 1.551(11) . ? C11 C12 1.377(10) . ? C11 H11 0.9300 . ? C12 C17 1.487(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.529(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C21 1.525(13) . ? C18 C19 1.537(12) . ? C18 C20 1.538(11) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C25 1.514(13) . ? C22 C23 1.515(12) . ? C22 C24 1.519(12) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C28 1.515(12) . ? C26 C29 1.531(11) . ? C26 C27 1.534(12) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31' 1.505(16) . ? C30 C33 1.521(16) . ? C30 C32 1.525(16) . ? C30 C32' 1.532(16) . ? C30 C33' 1.540(16) . ? C30 C31 1.556(16) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.506(17) . ? C40' C41' 1.506(17) . ? C41 C42 1.550(18) . ? C41' C42' 1.513(17) . ? C42 C43 1.521(17) . ? C42' C43' 1.500(17) . ? C44 C45 1.384(19) . ? C44 C49 1.440(19) . ? C44 C50 1.522(19) . ? C44' C45' 1.402(19) . ? C44' C49' 1.442(18) . ? C44' C50' 1.508(19) . ? C45 C46 1.430(19) . ? C45' C46' 1.413(19) . ? C46 C47 1.436(19) . ? C46' C47' 1.421(19) . ? C47 C48 1.427(19) . ? C47' C48' 1.389(19) . ? C48 C49 1.394(19) . ? C48' C49' 1.380(19) . ? 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 O2 111.06(19) . . ? O1 Nd1 N3 122.1(2) . . ? O2 Nd1 N3 125.8(2) . . ? O1 Nd1 O3 88.56(18) . . ? O2 Nd1 O3 85.66(19) . . ? N3 Nd1 O3 85.6(2) . . ? O1 Nd1 N1 70.88(17) . . ? O2 Nd1 N1 112.61(18) . . ? N3 Nd1 N1 94.9(2) . . ? O3 Nd1 N1 156.10(18) . . ? O1 Nd1 N2 109.90(17) . . ? O2 Nd1 N2 71.31(17) . . ? N3 Nd1 N2 98.5(2) . . ? O3 Nd1 N2 154.32(18) . . ? N1 Nd1 N2 49.26(17) . . ? O1 Nd1 C14 79.81(18) . . ? O2 Nd1 C14 82.71(19) . . ? N3 Nd1 C14 115.0(2) . . ? O3 Nd1 C14 159.3(2) . . ? N3 Si1 C36 115.7(5) . . ? N3 Si1 C34 110.1(4) . . ? C36 Si1 C34 105.7(6) . . ? N3 Si1 C35 113.6(5) . . ? C36 Si1 C35 105.6(7) . . ? C34 Si1 C35 105.2(6) . . ? N3 Si2 C39 114.4(5) . . ? N3 Si2 C37 110.7(4) . . ? C39 Si2 C37 105.5(7) . . ? N3 Si2 C38 114.2(5) . . ? C39 Si2 C38 106.1(8) . . ? C37 Si2 C38 105.2(7) . . ? C1 O1 Nd1 145.6(4) . . ? C7 O2 Nd1 141.1(4) . . ? C43' O3 C43 31.5(10) . . ? C43' O3 C40 98.9(13) . . ? C43 O3 C40 110.9(12) . . ? C43' O3 C40' 112.1(11) . . ? C43 O3 C40' 106.8(12) . . ? C40 O3 C40' 31.3(11) . . ? C43' O3 Nd1 134.2(9) . . ? C43 O3 Nd1 127.4(9) . . ? C40 O3 Nd1 121.3(9) . . ? C40' O3 Nd1 113.7(8) . . ? C14 N1 C13 116.1(6) . . ? C14 N1 C15 102.7(5) . . ? C13 N1 C15 111.8(5) . . ? C14 N1 Nd1 85.2(4) . . ? C13 N1 Nd1 125.4(4) . . ? C15 N1 Nd1 110.9(4) . . ? C14 N2 C17 116.0(6) . . ? C14 N2 C16 102.6(5) . . ? C17 N2 C16 113.9(5) . . ? C14 N2 Nd1 84.9(4) . . ? C17 N2 Nd1 123.6(4) . . ? C16 N2 Nd1 110.7(4) . . ? Si2 N3 Si1 122.5(4) . . ? Si2 N3 Nd1 118.1(4) . . ? Si1 N3 Nd1 119.1(3) . . ? O1 C1 C6 120.6(6) . . ? O1 C1 C2 121.3(6) . . ? C6 C1 C2 118.2(7) . . ? C3 C2 C1 117.9(7) . . ? C3 C2 C18 120.2(7) . . ? C1 C2 C18 121.9(7) . . ? C4 C3 C2 124.2(7) . . ? C4 C3 H3 117.9 . . ? C2 C3 H3 117.9 . . ? C5 C4 C3 115.9(7) . . ? C5 C4 C22 123.2(7) . . ? C3 C4 C22 120.7(7) . . ? C6 C5 C4 122.6(7) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C1 121.0(7) . . ? C5 C6 C13 115.8(6) . . ? C1 C6 C13 123.1(7) . . ? O2 C7 C12 119.9(7) . . ? O2 C7 C8 121.8(7) . . ? C12 C7 C8 118.3(7) . . ? C9 C8 C7 117.9(7) . . ? C9 C8 C26 120.7(7) . . ? C7 C8 C26 121.4(7) . . ? C10 C9 C8 124.7(7) . . ? C10 C9 H9 117.7 . . ? C8 C9 H9 117.7 . . ? C9 C10 C11 115.6(7) . . ? C9 C10 C30 123.2(7) . . ? C11 C10 C30 121.2(7) . . ? C12 C11 C10 123.4(7) . . ? C12 C11 H11 118.3 . . ? C10 C11 H11 118.3 . . ? C11 C12 C7 119.7(7) . . ? C11 C12 C17 118.4(7) . . ? C7 C12 C17 121.7(7) . . ? N1 C13 C6 115.9(6) . . ? N1 C13 H13A 108.3 . . ? C6 C13 H13A 108.3 . . ? N1 C13 H13B 108.3 . . ? C6 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? N1 C14 N2 97.9(5) . . ? N1 C14 H14A 112.2 . . ? N2 C14 H14A 112.2 . . ? N1 C14 H14B 112.2 . . ? N2 C14 H14B 112.2 . . ? H14A C14 H14B 109.8 . . ? N1 C15 C16 102.6(6) . . ? N1 C15 H15A 111.2 . . ? C16 C15 H15A 111.2 . . ? N1 C15 H15B 111.2 . . ? C16 C15 H15B 111.2 . . ? H15A C15 H15B 109.2 . . ? N2 C16 C15 103.0(5) . . ? N2 C16 H16A 111.2 . . ? C15 C16 H16A 111.2 . . ? N2 C16 H16B 111.2 . . ? C15 C16 H16B 111.2 . . ? H16A C16 H16B 109.1 . . ? N2 C17 C12 116.3(6) . . ? N2 C17 H17A 108.2 . . ? C12 C17 H17A 108.2 . . ? N2 C17 H17B 108.2 . . ? C12 C17 H17B 108.2 . . ? H17A C17 H17B 107.4 . . ? C21 C18 C19 107.5(7) . . ? C21 C18 C2 108.5(7) . . ? C19 C18 C2 112.7(7) . . ? C21 C18 C20 111.6(8) . . ? C19 C18 C20 107.0(8) . . ? C2 C18 C20 109.5(6) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C25 C22 C23 107.9(8) . . ? C25 C22 C24 107.6(9) . . ? C23 C22 C24 110.3(9) . . ? C25 C22 C4 111.5(7) . . ? C23 C22 C4 108.3(7) . . ? C24 C22 C4 111.1(7) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C28 C26 C29 110.9(7) . . ? C28 C26 C27 107.2(7) . . ? C29 C26 C27 107.1(7) . . ? C28 C26 C8 108.9(7) . . ? C29 C26 C8 110.4(6) . . ? C27 C26 C8 112.2(7) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31' C30 C33 66.1(13) . . ? C31' C30 C32 132.4(15) . . ? C33 C30 C32 111.6(15) . . ? C31' C30 C32' 116.5(15) . . ? C33 C30 C32' 137.7(15) . . ? C32 C30 C32' 32.6(11) . . ? C31' C30 C33' 101.5(15) . . ? C33 C30 C33' 39.7(11) . . ? C32 C30 C33' 74.7(14) . . ? C32' C30 C33' 106.1(15) . . ? C31' C30 C10 113.6(11) . . ? C33 C30 C10 107.5(11) . . ? C32 C30 C10 111.9(11) . . ? C32' C30 C10 108.7(11) . . ? C33' C30 C10 109.8(12) . . ? C31' C30 C31 41.3(11) . . ? C33 C30 C31 106.4(14) . . ? C32 C30 C31 108.9(15) . . ? C32' C30 C31 80.8(14) . . ? C33' C30 C31 134.2(15) . . ? C10 C30 C31 110.3(11) . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si2 C37 H37A 109.5 . . ? Si2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si2 C38 H38A 109.5 . . ? Si2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si2 C39 H39A 109.5 . . ? Si2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O3 C40 C41 104.3(16) . . ? O3 C40' C41' 106.1(14) . . ? C40 C41 C42 103.8(18) . . ? C40' C41' C42' 106.9(17) . . ? C43 C42 C41 101.3(18) . . ? C43' C42' C41' 109.1(18) . . ? O3 C43 C42 104.8(14) . . ? O3 C43' C42' 105.5(15) . . ? C45 C44 C49 118(3) . . ? C45 C44 C50 116(3) . . ? C49 C44 C50 124(3) . . ? C45' C44' C49' 114(2) . . ? C45' C44' C50' 128(3) . . ? C49' C44' C50' 116(2) . . ? C44 C45 C46 118(3) . . ? C44' C45' C46' 120(2) . . ? C45 C46 C47 125(3) . . ? C45' C46' C47' 123(3) . . ? C48 C47 C46 114(3) . . ? C48' C47' C46' 117(3) . . ? C49 C48 C47 121(3) . . ? C49' C48' C47' 118(2) . . ? C48 C49 C44 123(3) . . ? C48' C49' C44' 126(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.797 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.089 #===================================================end data_complex4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H76 N3 O3 Si2 Sm' _chemical_formula_sum 'C43 H76 N3 O3 Si2 Sm' _chemical_formula_weight 889.60 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' 'Sm' 'Sm' -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 10.3105(10) _cell_length_b 20.4977(19) _cell_length_c 22.631(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.160(2) _cell_angle_gamma 90.00 _cell_volume 4707.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13917 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1876 _exptl_absorpt_coefficient_mu 1.336 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.544 _exptl_absorpt_correction_T_max 0.697 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39410 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8481 _reflns_number_gt 7247 _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 ? _computing_publication_material ? _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^)+(0.0303P)^2^+7.6109P] 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 8481 _refine_ls_number_parameters 480 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.60858(2) 0.508699(10) 0.710372(9) 0.02472(8) Uani 1 1 d . . . Si1 Si 0.42936(14) 0.37743(7) 0.75512(7) 0.0451(4) Uani 1 1 d . . . Si2 Si 0.36906(13) 0.41106(7) 0.62407(6) 0.0405(3) Uani 1 1 d . . . O1 O 0.6321(3) 0.58286(14) 0.64221(13) 0.0322(7) Uani 1 1 d . . . O2 O 0.7166(3) 0.54068(14) 0.79792(13) 0.0331(7) Uani 1 1 d . . . O3 O 0.4170(3) 0.57664(16) 0.73021(14) 0.0421(8) Uani 1 1 d . . . N1 N 0.7782(3) 0.46382(16) 0.64682(15) 0.0255(8) Uani 1 1 d . . . N2 N 0.8139(3) 0.43384(16) 0.74136(15) 0.0258(8) Uani 1 1 d . . . N3 N 0.4559(3) 0.42232(17) 0.69480(16) 0.0323(9) Uani 1 1 d . . . C1 C 0.7218(4) 0.6087(2) 0.61234(18) 0.0269(9) Uani 1 1 d . . . C2 C 0.7211(4) 0.6761(2) 0.59798(18) 0.0276(10) Uani 1 1 d . . . C3 C 0.8248(4) 0.7000(2) 0.57260(19) 0.0303(10) Uani 1 1 d . . . H3 H 0.8263 0.7450 0.5647 0.036 Uiso 1 1 calc R . . C4 C 0.9267(4) 0.6621(2) 0.55798(19) 0.0293(10) Uani 1 1 d . . . C5 C 0.9179(4) 0.5960(2) 0.56811(18) 0.0284(10) Uani 1 1 d . . . H5 H 0.9827 0.5683 0.5574 0.034 Uiso 1 1 calc R . . C6 C 0.8171(4) 0.5685(2) 0.59344(18) 0.0265(9) Uani 1 1 d . . . C7 C 0.8328(4) 0.5425(2) 0.83547(18) 0.0266(9) Uani 1 1 d . . . C8 C 0.8693(4) 0.5956(2) 0.87530(18) 0.0298(10) Uani 1 1 d . . . C9 C 0.9937(4) 0.5944(2) 0.91146(19) 0.0346(11) Uani 1 1 d . . . H9 H 1.0173 0.6298 0.9376 0.042 Uiso 1 1 calc R . . C10 C 1.0850(4) 0.5446(2) 0.91152(18) 0.0331(10) Uani 1 1 d . . . C11 C 1.0459(4) 0.4928(2) 0.87337(18) 0.0306(10) Uani 1 1 d . . . H11 H 1.1046 0.4578 0.8724 0.037 Uiso 1 1 calc R . . C12 C 0.9218(4) 0.4905(2) 0.83613(18) 0.0274(9) Uani 1 1 d . . . C13 C 0.8068(4) 0.49500(19) 0.59214(19) 0.0301(10) Uani 1 1 d . . . H13A H 0.7374 0.4826 0.5586 0.036 Uiso 1 1 calc R . . H13B H 0.8899 0.4772 0.5838 0.036 Uiso 1 1 calc R . . C14 C 0.8752(4) 0.4754(2) 0.70148(18) 0.0261(9) Uani 1 1 d . . . H14A H 0.9635 0.4603 0.6977 0.031 Uiso 1 1 calc R . . H14B H 0.8786 0.5213 0.7138 0.031 Uiso 1 1 calc R . . C15 C 0.7733(4) 0.39149(19) 0.64355(19) 0.0318(10) Uani 1 1 d . . . H15A H 0.8418 0.3743 0.6228 0.038 Uiso 1 1 calc R . . H15B H 0.6870 0.3763 0.6228 0.038 Uiso 1 1 calc R . . C16 C 0.7977(4) 0.3713(2) 0.70903(19) 0.0314(10) Uani 1 1 d . . . H16A H 0.7226 0.3468 0.7188 0.038 Uiso 1 1 calc R . . H16B H 0.8773 0.3445 0.7187 0.038 Uiso 1 1 calc R . . C17 C 0.8864(4) 0.4271(2) 0.80314(19) 0.0311(10) Uani 1 1 d . . . H17A H 0.9678 0.4028 0.8020 0.037 Uiso 1 1 calc R . . H17B H 0.8330 0.4010 0.8261 0.037 Uiso 1 1 calc R . . C18 C 0.6064(4) 0.7205(2) 0.60649(19) 0.0302(10) Uani 1 1 d . . . C19 C 0.6190(5) 0.7892(2) 0.5820(2) 0.0429(12) Uani 1 1 d . . . H19A H 0.6996 0.8092 0.6028 0.064 Uiso 1 1 calc R . . H19B H 0.5441 0.8153 0.5882 0.064 Uiso 1 1 calc R . . H19C H 0.6215 0.7869 0.5394 0.064 Uiso 1 1 calc R . . C20 C 0.5981(5) 0.7272(2) 0.6733(2) 0.0456(13) Uani 1 1 d . . . H20A H 0.5864 0.6844 0.6899 0.068 Uiso 1 1 calc R . . H20B H 0.5238 0.7547 0.6776 0.068 Uiso 1 1 calc R . . H20C H 0.6787 0.7467 0.6946 0.068 Uiso 1 1 calc R . . C21 C 0.4782(4) 0.6921(2) 0.5710(2) 0.0399(12) Uani 1 1 d . . . H21A H 0.4812 0.6934 0.5284 0.060 Uiso 1 1 calc R . . H21B H 0.4039 0.7176 0.5789 0.060 Uiso 1 1 calc R . . H21C H 0.4684 0.6473 0.5833 0.060 Uiso 1 1 calc R . . C22 C 1.0358(4) 0.6940(2) 0.5298(2) 0.0331(10) Uani 1 1 d . . . C23 C 1.1029(5) 0.7485(3) 0.5702(3) 0.0541(15) Uani 1 1 d . . . H23A H 1.1381 0.7309 0.6095 0.081 Uiso 1 1 calc R . . H23B H 1.0392 0.7823 0.5740 0.081 Uiso 1 1 calc R . . H23C H 1.1741 0.7668 0.5526 0.081 Uiso 1 1 calc R . . C24 C 0.9758(5) 0.7231(3) 0.4687(2) 0.0526(14) Uani 1 1 d . . . H24A H 1.0454 0.7413 0.4499 0.079 Uiso 1 1 calc R . . H24B H 0.9140 0.7572 0.4742 0.079 Uiso 1 1 calc R . . H24C H 0.9302 0.6892 0.4432 0.079 Uiso 1 1 calc R . . C25 C 1.1403(5) 0.6446(2) 0.5193(2) 0.0428(12) Uani 1 1 d . . . H25A H 1.2073 0.6664 0.5014 0.064 Uiso 1 1 calc R . . H25B H 1.0995 0.6105 0.4926 0.064 Uiso 1 1 calc R . . H25C H 1.1805 0.6255 0.5574 0.064 Uiso 1 1 calc R . . C26 C 0.7717(5) 0.6504(2) 0.8814(2) 0.0352(11) Uani 1 1 d . . . C27 C 0.8296(6) 0.7014(3) 0.9284(3) 0.0591(16) Uani 1 1 d . . . H27A H 0.8523 0.6806 0.9674 0.089 Uiso 1 1 calc R . . H27B H 0.7649 0.7354 0.9303 0.089 Uiso 1 1 calc R . . H27C H 0.9080 0.7204 0.9173 0.089 Uiso 1 1 calc R . . C28 C 0.6504(5) 0.6214(2) 0.9023(2) 0.0473(13) Uani 1 1 d . . . H28A H 0.6148 0.5864 0.8754 0.071 Uiso 1 1 calc R . . H28B H 0.5842 0.6550 0.9020 0.071 Uiso 1 1 calc R . . H28C H 0.6755 0.6043 0.9427 0.071 Uiso 1 1 calc R . . C29 C 0.7321(6) 0.6858(3) 0.8216(2) 0.0602(16) Uani 1 1 d . . . H29A H 0.8093 0.7060 0.8104 0.090 Uiso 1 1 calc R . . H29B H 0.6673 0.7190 0.8255 0.090 Uiso 1 1 calc R . . H29C H 0.6948 0.6547 0.7909 0.090 Uiso 1 1 calc R . . C30 C 1.2174(4) 0.5467(2) 0.9549(2) 0.0398(12) Uani 1 1 d . . . C31 C 1.2895(5) 0.6110(3) 0.9481(3) 0.0636(17) Uani 1 1 d . . . H31A H 1.3728 0.6115 0.9758 0.095 Uiso 1 1 calc R . . H31B H 1.2356 0.6473 0.9568 0.095 Uiso 1 1 calc R . . H31C H 1.3058 0.6148 0.9073 0.095 Uiso 1 1 calc R . . C32 C 1.3075(5) 0.4905(3) 0.9434(3) 0.0634(17) Uani 1 1 d . . . H32A H 1.2675 0.4493 0.9512 0.095 Uiso 1 1 calc R . . H32B H 1.3922 0.4949 0.9697 0.095 Uiso 1 1 calc R . . H32C H 1.3199 0.4918 0.9019 0.095 Uiso 1 1 calc R . . C33 C 1.1921(5) 0.5414(3) 1.0194(2) 0.0476(13) Uani 1 1 d . . . H33A H 1.1473 0.5007 1.0243 0.071 Uiso 1 1 calc R . . H33B H 1.1375 0.5777 1.0277 0.071 Uiso 1 1 calc R . . H33C H 1.2754 0.5426 1.0471 0.071 Uiso 1 1 calc R . . C34 C 0.5275(6) 0.4103(3) 0.8268(2) 0.0653(17) Uani 1 1 d . . . H34A H 0.6207 0.4075 0.8252 0.098 Uiso 1 1 calc R . . H34B H 0.5087 0.3849 0.8604 0.098 Uiso 1 1 calc R . . H34C H 0.5036 0.4555 0.8317 0.098 Uiso 1 1 calc R . . C35 C 0.4799(7) 0.2901(3) 0.7540(3) 0.079(2) Uani 1 1 d . . . H35A H 0.4280 0.2684 0.7196 0.119 Uiso 1 1 calc R . . H35B H 0.4655 0.2688 0.7906 0.119 Uiso 1 1 calc R . . H35C H 0.5726 0.2875 0.7511 0.119 Uiso 1 1 calc R . . C36 C 0.2527(6) 0.3761(4) 0.7662(3) 0.086(2) Uani 1 1 d . . . H36A H 0.2192 0.4204 0.7653 0.130 Uiso 1 1 calc R . . H36B H 0.2476 0.3564 0.8047 0.130 Uiso 1 1 calc R . . H36C H 0.2004 0.3509 0.7343 0.130 Uiso 1 1 calc R . . C37 C 0.1885(5) 0.4321(3) 0.6149(3) 0.0654(17) Uani 1 1 d . . . H37A H 0.1449 0.4013 0.6375 0.098 Uiso 1 1 calc R . . H37B H 0.1489 0.4298 0.5728 0.098 Uiso 1 1 calc R . . H37C H 0.1788 0.4759 0.6297 0.098 Uiso 1 1 calc R . . C38 C 0.4329(6) 0.4652(3) 0.5687(3) 0.0699(18) Uani 1 1 d . . . H38A H 0.4335 0.5101 0.5823 0.105 Uiso 1 1 calc R . . H38B H 0.3763 0.4614 0.5298 0.105 Uiso 1 1 calc R . . H38C H 0.5217 0.4520 0.5655 0.105 Uiso 1 1 calc R . . C39 C 0.3769(6) 0.3263(3) 0.5952(3) 0.0651(17) Uani 1 1 d . . . H39A H 0.4682 0.3125 0.6002 0.098 Uiso 1 1 calc R . . H39B H 0.3377 0.3251 0.5530 0.098 Uiso 1 1 calc R . . H39C H 0.3290 0.2972 0.6175 0.098 Uiso 1 1 calc R . . C40 C 0.3813(12) 0.5996(7) 0.7874(6) 0.063(3) Uiso 0.50 1 d PD . . C40' C 0.3503(12) 0.5628(7) 0.7808(6) 0.061(3) Uiso 0.50 1 d PD . . C41 C 0.2408(12) 0.6220(7) 0.7716(5) 0.063(3) Uiso 0.50 1 d PD . . C41' C 0.2120(13) 0.5883(7) 0.7665(6) 0.072(4) Uiso 0.50 1 d PD . . C42 C 0.1886(10) 0.5982(6) 0.7074(5) 0.052(3) Uiso 0.50 1 d PD . . C42' C 0.2053(15) 0.6298(8) 0.7106(7) 0.091(5) Uiso 0.50 1 d PD . . C43 C 0.3173(7) 0.6020(3) 0.6818(3) 0.0772(19) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02155(13) 0.02671(13) 0.02586(13) 0.00082(9) 0.00407(9) -0.00010(9) Si1 0.0381(8) 0.0472(9) 0.0524(9) 0.0010(7) 0.0151(7) -0.0115(6) Si2 0.0264(7) 0.0453(8) 0.0474(8) -0.0092(6) 0.0004(6) -0.0031(6) O1 0.0307(17) 0.0314(17) 0.0369(17) 0.0072(14) 0.0130(14) 0.0029(13) O2 0.0318(17) 0.0337(17) 0.0316(16) -0.0056(14) -0.0004(14) 0.0051(13) O3 0.0341(19) 0.052(2) 0.0419(19) 0.0069(16) 0.0103(15) 0.0138(15) N1 0.0271(19) 0.0228(18) 0.0268(18) 0.0000(15) 0.0048(15) 0.0006(15) N2 0.028(2) 0.0215(18) 0.0277(19) -0.0019(15) 0.0035(16) -0.0004(14) N3 0.028(2) 0.032(2) 0.037(2) -0.0040(17) 0.0061(17) -0.0054(16) C1 0.022(2) 0.030(2) 0.029(2) 0.0031(19) 0.0035(18) -0.0009(18) C2 0.027(2) 0.031(2) 0.024(2) 0.0009(18) 0.0029(19) 0.0017(18) C3 0.033(3) 0.026(2) 0.032(2) 0.0000(19) 0.004(2) -0.0025(19) C4 0.026(2) 0.033(2) 0.029(2) 0.0019(19) 0.0044(19) -0.0047(19) C5 0.022(2) 0.033(2) 0.031(2) -0.0027(19) 0.0056(19) 0.0055(18) C6 0.028(2) 0.028(2) 0.024(2) 0.0022(18) 0.0052(19) 0.0032(18) C7 0.023(2) 0.033(2) 0.024(2) 0.0032(18) 0.0036(18) 0.0007(18) C8 0.035(3) 0.030(2) 0.025(2) -0.0024(19) 0.007(2) -0.0011(19) C9 0.039(3) 0.037(3) 0.029(2) -0.007(2) 0.008(2) -0.006(2) C10 0.031(3) 0.045(3) 0.023(2) -0.001(2) 0.0056(19) -0.007(2) C11 0.030(2) 0.035(3) 0.027(2) 0.0021(19) 0.0061(19) 0.0028(19) C12 0.029(2) 0.030(2) 0.024(2) 0.0029(18) 0.0068(18) 0.0007(18) C13 0.032(2) 0.029(2) 0.030(2) 0.0001(19) 0.0098(19) 0.0026(19) C14 0.023(2) 0.024(2) 0.031(2) -0.0016(18) 0.0046(18) 0.0022(17) C15 0.036(3) 0.023(2) 0.037(3) -0.0072(19) 0.008(2) -0.0025(19) C16 0.034(3) 0.023(2) 0.037(3) 0.0010(19) 0.006(2) -0.0024(18) C17 0.034(3) 0.026(2) 0.034(2) 0.0056(19) 0.006(2) 0.0083(19) C18 0.030(2) 0.027(2) 0.034(2) 0.0041(19) 0.009(2) 0.0050(18) C19 0.042(3) 0.030(3) 0.057(3) 0.005(2) 0.012(3) 0.009(2) C20 0.055(3) 0.047(3) 0.037(3) -0.001(2) 0.013(2) 0.014(2) C21 0.027(3) 0.043(3) 0.049(3) 0.005(2) 0.005(2) 0.007(2) C22 0.024(2) 0.035(3) 0.040(3) 0.003(2) 0.007(2) -0.0040(19) C23 0.041(3) 0.053(3) 0.072(4) -0.019(3) 0.022(3) -0.018(3) C24 0.039(3) 0.064(4) 0.057(3) 0.021(3) 0.014(3) -0.011(3) C25 0.034(3) 0.050(3) 0.048(3) -0.003(2) 0.017(2) -0.008(2) C26 0.040(3) 0.028(2) 0.037(3) -0.004(2) 0.006(2) 0.001(2) C27 0.053(4) 0.046(3) 0.078(4) -0.029(3) 0.008(3) -0.002(3) C28 0.040(3) 0.042(3) 0.061(3) -0.010(3) 0.013(3) 0.005(2) C29 0.082(4) 0.036(3) 0.063(4) 0.008(3) 0.015(3) 0.014(3) C30 0.027(3) 0.057(3) 0.034(3) -0.006(2) 0.001(2) -0.007(2) C31 0.044(3) 0.087(5) 0.058(4) -0.002(3) 0.004(3) -0.026(3) C32 0.034(3) 0.094(5) 0.057(4) -0.018(3) -0.009(3) 0.015(3) C33 0.041(3) 0.066(4) 0.032(3) 0.000(2) -0.003(2) 0.000(3) C34 0.060(4) 0.084(5) 0.051(3) 0.005(3) 0.011(3) -0.012(3) C35 0.100(5) 0.050(4) 0.095(5) 0.013(4) 0.035(4) -0.012(4) C36 0.047(4) 0.132(7) 0.088(5) 0.022(5) 0.034(4) -0.019(4) C37 0.036(3) 0.075(4) 0.080(4) -0.013(3) -0.006(3) 0.001(3) C38 0.053(4) 0.102(5) 0.051(4) 0.014(4) -0.001(3) -0.014(3) C39 0.053(4) 0.063(4) 0.075(4) -0.031(3) 0.000(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O2 2.195(3) . ? Sm1 O1 2.209(3) . ? Sm1 N3 2.354(3) . ? Sm1 O3 2.521(3) . ? Sm1 N2 2.608(3) . ? Sm1 N1 2.620(3) . ? Sm1 C14 2.874(4) . ? Si1 N3 1.708(4) . ? Si1 C35 1.867(6) . ? Si1 C34 1.878(6) . ? Si1 C36 1.882(6) . ? Si2 N3 1.706(4) . ? Si2 C39 1.863(5) . ? Si2 C38 1.876(6) . ? Si2 C37 1.886(5) . ? O1 C1 1.346(5) . ? O2 C7 1.342(5) . ? O3 C43 1.460(7) . ? O3 C40' 1.464(13) . ? O3 C40 1.483(13) . ? N1 C14 1.466(5) . ? N1 C13 1.468(5) . ? N1 C15 1.485(5) . ? N2 C14 1.463(5) . ? N2 C17 1.471(5) . ? N2 C16 1.471(5) . ? C1 C6 1.406(6) . ? C1 C2 1.420(6) . ? C2 C3 1.389(6) . ? C2 C18 1.531(6) . ? C3 C4 1.393(6) . ? C3 H3 0.9400 . ? C4 C5 1.380(6) . ? C4 C22 1.534(6) . ? C5 C6 1.391(6) . ? C5 H5 0.9400 . ? C6 C13 1.510(6) . ? C7 C12 1.406(6) . ? C7 C8 1.420(6) . ? C8 C9 1.395(6) . ? C8 C26 1.531(6) . ? C9 C10 1.388(6) . ? C9 H9 0.9400 . ? C10 C11 1.384(6) . ? C10 C30 1.535(6) . ? C11 C12 1.403(6) . ? C11 H11 0.9400 . ? C12 C17 1.511(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.516(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 C19 1.527(6) . ? C18 C21 1.536(6) . ? C18 C20 1.536(6) . ? 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 C25 1.527(6) . ? C22 C23 1.529(6) . ? C22 C24 1.533(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 C29 1.527(7) . ? C26 C28 1.532(7) . ? C26 C27 1.535(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 C32 1.531(7) . ? C30 C33 1.531(6) . ? C30 C31 1.535(7) . ? 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 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? 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 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C40 C41 1.502(13) . ? C40' C41' 1.500(13) . ? C41 C42 1.538(13) . ? C41' C42' 1.516(15) . ? C42 C43 1.540(11) . ? C42' C43 1.532(13) . ? 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 O2 Sm1 O1 108.90(11) . . ? O2 Sm1 N3 125.40(12) . . ? O1 Sm1 N3 124.47(12) . . ? O2 Sm1 O3 87.88(10) . . ? O1 Sm1 O3 86.00(10) . . ? N3 Sm1 O3 85.28(12) . . ? O2 Sm1 N2 71.00(10) . . ? O1 Sm1 N2 114.11(10) . . ? N3 Sm1 N2 95.02(11) . . ? O3 Sm1 N2 154.33(10) . . ? O2 Sm1 N1 108.60(10) . . ? O1 Sm1 N1 72.06(10) . . ? N3 Sm1 N1 98.48(11) . . ? O3 Sm1 N1 155.76(10) . . ? N2 Sm1 N1 49.63(10) . . ? O2 Sm1 C14 78.16(11) . . ? O1 Sm1 C14 83.69(11) . . ? N3 Sm1 C14 115.71(12) . . ? O3 Sm1 C14 158.88(11) . . ? N2 Sm1 C14 30.48(11) . . ? N1 Sm1 C14 30.52(10) . . ? N3 Si1 C35 114.9(2) . . ? N3 Si1 C34 111.0(2) . . ? C35 Si1 C34 104.3(3) . . ? N3 Si1 C36 114.2(3) . . ? C35 Si1 C36 105.5(3) . . ? C34 Si1 C36 106.1(3) . . ? N3 Si2 C39 114.0(2) . . ? N3 Si2 C38 111.0(2) . . ? C39 Si2 C38 106.0(3) . . ? N3 Si2 C37 114.6(2) . . ? C39 Si2 C37 106.1(3) . . ? C38 Si2 C37 104.3(3) . . ? C1 O1 Sm1 142.3(3) . . ? C7 O2 Sm1 146.6(3) . . ? C43 O3 C40' 106.9(6) . . ? C43 O3 C40 107.0(6) . . ? C40' O3 C40 32.4(6) . . ? C43 O3 Sm1 122.2(3) . . ? C40' O3 Sm1 121.6(5) . . ? C40 O3 Sm1 130.8(5) . . ? C14 N1 C13 115.6(3) . . ? C14 N1 C15 102.5(3) . . ? C13 N1 C15 113.8(3) . . ? C14 N1 Sm1 84.4(2) . . ? C13 N1 Sm1 124.2(2) . . ? C15 N1 Sm1 110.9(2) . . ? C14 N2 C17 116.0(3) . . ? C14 N2 C16 103.0(3) . . ? C17 N2 C16 112.6(3) . . ? C14 N2 Sm1 84.8(2) . . ? C17 N2 Sm1 124.3(2) . . ? C16 N2 Sm1 111.3(2) . . ? Si2 N3 Si1 123.1(2) . . ? Si2 N3 Sm1 117.94(18) . . ? Si1 N3 Sm1 118.86(18) . . ? O1 C1 C6 120.1(4) . . ? O1 C1 C2 121.4(4) . . ? C6 C1 C2 118.5(4) . . ? C3 C2 C1 117.7(4) . . ? C3 C2 C18 120.7(4) . . ? C1 C2 C18 121.5(4) . . ? C2 C3 C4 124.7(4) . . ? C2 C3 H3 117.7 . . ? C4 C3 H3 117.7 . . ? C5 C4 C3 115.7(4) . . ? C5 C4 C22 124.2(4) . . ? C3 C4 C22 120.0(4) . . ? C4 C5 C6 122.8(4) . . ? C4 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C5 C6 C1 120.1(4) . . ? C5 C6 C13 116.8(4) . . ? C1 C6 C13 122.6(4) . . ? O2 C7 C12 119.6(4) . . ? O2 C7 C8 122.0(4) . . ? C12 C7 C8 118.4(4) . . ? C9 C8 C7 118.2(4) . . ? C9 C8 C26 120.7(4) . . ? C7 C8 C26 121.0(4) . . ? C10 C9 C8 124.5(4) . . ? C10 C9 H9 117.8 . . ? C8 C9 H9 117.8 . . ? C11 C10 C9 116.2(4) . . ? C11 C10 C30 123.3(4) . . ? C9 C10 C30 120.4(4) . . ? C10 C11 C12 122.4(4) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C11 C12 C7 120.3(4) . . ? C11 C12 C17 116.2(4) . . ? C7 C12 C17 123.2(4) . . ? N1 C13 C6 116.2(3) . . ? N1 C13 H13A 108.2 . . ? C6 C13 H13A 108.2 . . ? N1 C13 H13B 108.2 . . ? C6 C13 H13B 108.2 . . ? H13A C13 H13B 107.4 . . ? N2 C14 N1 97.0(3) . . ? N2 C14 Sm1 64.68(19) . . ? N1 C14 Sm1 65.11(19) . . ? N2 C14 H14A 112.4 . . ? N1 C14 H14A 112.4 . . ? Sm1 C14 H14A 175.2 . . ? N2 C14 H14B 112.4 . . ? N1 C14 H14B 112.4 . . ? Sm1 C14 H14B 74.8 . . ? H14A C14 H14B 109.9 . . ? N1 C15 C16 103.0(3) . . ? N1 C15 H15A 111.2 . . ? C16 C15 H15A 111.2 . . ? N1 C15 H15B 111.2 . . ? C16 C15 H15B 111.2 . . ? H15A C15 H15B 109.1 . . ? N2 C16 C15 103.5(3) . . ? N2 C16 H16A 111.1 . . ? C15 C16 H16A 111.1 . . ? N2 C16 H16B 111.1 . . ? C15 C16 H16B 111.1 . . ? H16A C16 H16B 109.0 . . ? N2 C17 C12 115.3(3) . . ? N2 C17 H17A 108.5 . . ? C12 C17 H17A 108.5 . . ? N2 C17 H17B 108.5 . . ? C12 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C19 C18 C2 112.7(4) . . ? C19 C18 C21 106.3(4) . . ? C2 C18 C21 108.7(4) . . ? C19 C18 C20 107.4(4) . . ? C2 C18 C20 110.8(4) . . ? C21 C18 C20 110.8(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C25 C22 C23 108.6(4) . . ? C25 C22 C24 107.6(4) . . ? C23 C22 C24 108.8(4) . . ? C25 C22 C4 111.8(4) . . ? C23 C22 C4 110.5(4) . . ? C24 C22 C4 109.5(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C29 C26 C8 110.2(4) . . ? C29 C26 C28 110.7(4) . . ? C8 C26 C28 109.2(4) . . ? C29 C26 C27 107.5(4) . . ? C8 C26 C27 112.4(4) . . ? C28 C26 C27 106.8(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C30 C33 108.7(4) . . ? C32 C30 C31 108.0(4) . . ? C33 C30 C31 108.9(4) . . ? C32 C30 C10 111.6(4) . . ? C33 C30 C10 109.0(4) . . ? C31 C30 C10 110.6(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 . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si2 C37 H37A 109.5 . . ? Si2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si2 C38 H38A 109.5 . . ? Si2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si2 C39 H39A 109.5 . . ? Si2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O3 C40 C41 105.5(9) . . ? O3 C40' C41' 108.9(9) . . ? C40 C41 C42 106.8(10) . . ? C40' C41' C42' 106.1(11) . . ? C41 C42 C43 99.1(8) . . ? C41' C42' C43 102.7(10) . . ? O3 C43 C42' 107.3(7) . . ? O3 C43 C42 103.8(6) . . ? C42' C43 C42 25.3(7) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.279 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.093 #===================================================end data_complex5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H76 N3 O3 Si2 Yb, C7 H8' _chemical_formula_sum 'C50 H84 N3 O3 Si2 Yb' _chemical_formula_weight 1004.42 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' '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' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 14.5090(18) _cell_length_b 32.814(4) _cell_length_c 12.0587(15) _cell_angle_alpha 90.00 _cell_angle_beta 111.367(2) _cell_angle_gamma 90.00 _cell_volume 5346.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 15869 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2108 _exptl_absorpt_coefficient_mu 1.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.514 _exptl_absorpt_correction_T_max 0.693 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46446 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.34 _reflns_number_total 9757 _reflns_number_gt 8374 _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 ? _computing_publication_material ? _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^)+(0.0256P)^2^+17.1628P] 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 9757 _refine_ls_number_parameters 511 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1110 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.182 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.596966(18) 0.639876(7) 0.80888(2) 0.02605(9) Uani 1 1 d . . . Si1 Si 0.81107(13) 0.69087(6) 0.86033(19) 0.0471(5) Uani 1 1 d . . . Si2 Si 0.81252(13) 0.63964(6) 1.06471(18) 0.0462(5) Uani 1 1 d . . . O1 O 0.5183(3) 0.65948(11) 0.6304(3) 0.0306(9) Uani 1 1 d . . . O2 O 0.5280(3) 0.58630(12) 0.8405(3) 0.0316(9) Uani 1 1 d . . . O3 O 0.6794(3) 0.59284(13) 0.7249(4) 0.0422(11) Uani 1 1 d . . . N1 N 0.5211(3) 0.70729(13) 0.8241(4) 0.0263(10) Uani 1 1 d . . . N2 N 0.5148(3) 0.66058(14) 0.9497(4) 0.0277(10) Uani 1 1 d . . . N3 N 0.7505(3) 0.65917(15) 0.9243(5) 0.0355(12) Uani 1 1 d . . . C1 C 0.4445(4) 0.68354(17) 0.5620(5) 0.0271(12) Uani 1 1 d . . . C2 C 0.3889(4) 0.67360(17) 0.4410(5) 0.0294(13) Uani 1 1 d . . . C3 C 0.3080(4) 0.69809(18) 0.3779(5) 0.0332(14) Uani 1 1 d . . . H3 H 0.2709 0.6912 0.2984 0.040 Uiso 1 1 calc R . . C4 C 0.2789(4) 0.73214(17) 0.4257(5) 0.0303(13) Uani 1 1 d . . . C5 C 0.3385(4) 0.74272(16) 0.5409(5) 0.0282(13) Uani 1 1 d . . . H5 H 0.3231 0.7664 0.5746 0.034 Uiso 1 1 calc R . . C6 C 0.4199(4) 0.71983(17) 0.6084(5) 0.0277(12) Uani 1 1 d . . . C7 C 0.4460(4) 0.57504(17) 0.8582(5) 0.0289(13) Uani 1 1 d . . . C8 C 0.3949(4) 0.53807(16) 0.8107(5) 0.0290(13) Uani 1 1 d . . . C9 C 0.3043(4) 0.53078(18) 0.8213(5) 0.0348(14) Uani 1 1 d . . . H9 H 0.2698 0.5070 0.7861 0.042 Uiso 1 1 calc R . . C10 C 0.2609(4) 0.55650(17) 0.8810(5) 0.0309(13) Uani 1 1 d . . . C11 C 0.3166(4) 0.59027(17) 0.9353(5) 0.0310(13) Uani 1 1 d . . . H11 H 0.2914 0.6080 0.9785 0.037 Uiso 1 1 calc R . . C12 C 0.4075(4) 0.59883(16) 0.9285(5) 0.0269(12) Uani 1 1 d . . . C13 C 0.4824(4) 0.73701(17) 0.7289(5) 0.0324(13) Uani 1 1 d . . . H13A H 0.5382 0.7518 0.7207 0.039 Uiso 1 1 calc R . . H13B H 0.4424 0.7568 0.7526 0.039 Uiso 1 1 calc R . . C14 C 0.4465(4) 0.68265(17) 0.8470(5) 0.0276(12) Uani 1 1 d . . . H14A H 0.4114 0.6645 0.7804 0.033 Uiso 1 1 calc R . . H14B H 0.3989 0.6992 0.8676 0.033 Uiso 1 1 calc R . . C15 C 0.5747(4) 0.72704(17) 0.9419(5) 0.0319(13) Uani 1 1 d . . . H15A H 0.5420 0.7523 0.9507 0.038 Uiso 1 1 calc R . . H15B H 0.6437 0.7329 0.9528 0.038 Uiso 1 1 calc R . . C16 C 0.5676(4) 0.69418(17) 1.0288(5) 0.0331(14) Uani 1 1 d . . . H16A H 0.6335 0.6855 1.0820 0.040 Uiso 1 1 calc R . . H16B H 0.5303 0.7041 1.0767 0.040 Uiso 1 1 calc R . . C17 C 0.4675(4) 0.63251(17) 1.0065(5) 0.0329(13) Uani 1 1 d . . . H17A H 0.4241 0.6483 1.0364 0.039 Uiso 1 1 calc R . . H17B H 0.5190 0.6202 1.0754 0.039 Uiso 1 1 calc R . . C18 C 0.4183(5) 0.63826(18) 0.3775(5) 0.0381(15) Uani 1 1 d . . . C19 C 0.3479(6) 0.6330(2) 0.2490(6) 0.055(2) Uani 1 1 d . . . H19A H 0.2817 0.6275 0.2474 0.083 Uiso 1 1 calc R . . H19B H 0.3699 0.6105 0.2129 0.083 Uiso 1 1 calc R . . H19C H 0.3471 0.6578 0.2048 0.083 Uiso 1 1 calc R . . C20 C 0.5216(5) 0.64713(19) 0.3753(6) 0.0453(17) Uani 1 1 d . . . H20A H 0.5180 0.6703 0.3239 0.068 Uiso 1 1 calc R . . H20B H 0.5452 0.6235 0.3453 0.068 Uiso 1 1 calc R . . H20C H 0.5669 0.6532 0.4553 0.068 Uiso 1 1 calc R . . C21 C 0.4171(5) 0.59801(19) 0.4410(6) 0.0461(17) Uani 1 1 d . . . H21A H 0.4579 0.6005 0.5247 0.069 Uiso 1 1 calc R . . H21B H 0.4429 0.5764 0.4056 0.069 Uiso 1 1 calc R . . H21C H 0.3497 0.5916 0.4330 0.069 Uiso 1 1 calc R . . C22 C 0.1833(4) 0.75508(19) 0.3548(5) 0.0357(14) Uani 1 1 d . . . C23 C 0.0967(5) 0.7310(2) 0.3645(7) 0.061(2) Uani 1 1 d . . . H23A H 0.0937 0.7044 0.3279 0.091 Uiso 1 1 calc R . . H23B H 0.0355 0.7456 0.3240 0.091 Uiso 1 1 calc R . . H23C H 0.1059 0.7276 0.4477 0.091 Uiso 1 1 calc R . . C24 C 0.1702(6) 0.7586(3) 0.2237(6) 0.063(2) Uani 1 1 d . . . H24A H 0.2272 0.7722 0.2170 0.094 Uiso 1 1 calc R . . H24B H 0.1109 0.7741 0.1816 0.094 Uiso 1 1 calc R . . H24C H 0.1642 0.7315 0.1892 0.094 Uiso 1 1 calc R . . C25 C 0.1817(5) 0.7981(2) 0.4012(7) 0.0534(19) Uani 1 1 d . . . H25A H 0.1836 0.7968 0.4824 0.080 Uiso 1 1 calc R . . H25B H 0.1217 0.8118 0.3514 0.080 Uiso 1 1 calc R . . H25C H 0.2389 0.8130 0.3995 0.080 Uiso 1 1 calc R . . C26 C 0.4423(5) 0.50558(17) 0.7560(5) 0.0368(15) Uani 1 1 d . . . C27 C 0.3771(6) 0.46746(19) 0.7163(7) 0.058(2) Uani 1 1 d . . . H27A H 0.3119 0.4753 0.6620 0.087 Uiso 1 1 calc R . . H27B H 0.3715 0.4542 0.7855 0.087 Uiso 1 1 calc R . . H27C H 0.4068 0.4488 0.6765 0.087 Uiso 1 1 calc R . . C28 C 0.5396(5) 0.4920(2) 0.8511(6) 0.0513(19) Uani 1 1 d . . . H28A H 0.5762 0.4753 0.8147 0.077 Uiso 1 1 calc R . . H28B H 0.5259 0.4762 0.9114 0.077 Uiso 1 1 calc R . . H28C H 0.5786 0.5157 0.8877 0.077 Uiso 1 1 calc R . . C29 C 0.4590(5) 0.52175(19) 0.6462(6) 0.0449(17) Uani 1 1 d . . . H29A H 0.4877 0.5005 0.6132 0.067 Uiso 1 1 calc R . . H29B H 0.5037 0.5449 0.6684 0.067 Uiso 1 1 calc R . . H29C H 0.3962 0.5302 0.5871 0.067 Uiso 1 1 calc R . . C30 C 0.1598(5) 0.54770(19) 0.8898(6) 0.0419(16) Uani 1 1 d D . . C31 C 0.0983(10) 0.5871(4) 0.8699(13) 0.073(4) Uiso 0.65 1 d P . . C31' C 0.080(2) 0.5742(9) 0.800(3) 0.079(8) Uiso 0.35 1 d P . . C32 C 0.1758(11) 0.5305(5) 1.0129(13) 0.081(4) Uiso 0.65 1 d P . . C32' C 0.157(2) 0.5627(9) 1.0099(19) 0.090(9) Uiso 0.35 1 d PD . . C33 C 0.1004(10) 0.5164(4) 0.7961(12) 0.077(4) Uiso 0.65 1 d PD . . C33' C 0.144(2) 0.5018(8) 0.908(2) 0.079(7) Uiso 0.35 1 d P . . C34 C 0.7248(6) 0.7130(3) 0.7181(8) 0.072(3) Uani 1 1 d . . . H34A H 0.6816 0.6918 0.6710 0.108 Uiso 1 1 calc R . . H34B H 0.7626 0.7246 0.6739 0.108 Uiso 1 1 calc R . . H34C H 0.6853 0.7342 0.7353 0.108 Uiso 1 1 calc R . . C35 C 0.9085(6) 0.6650(3) 0.8184(9) 0.080(3) Uani 1 1 d . . . H35A H 0.9646 0.6584 0.8899 0.120 Uiso 1 1 calc R . . H35B H 0.9297 0.6830 0.7685 0.120 Uiso 1 1 calc R . . H35C H 0.8817 0.6401 0.7751 0.120 Uiso 1 1 calc R . . C36 C 0.8728(7) 0.7355(3) 0.9555(9) 0.088(3) Uani 1 1 d . . . H36A H 0.8243 0.7507 0.9767 0.131 Uiso 1 1 calc R . . H36B H 0.9013 0.7530 0.9116 0.131 Uiso 1 1 calc R . . H36C H 0.9246 0.7259 1.0272 0.131 Uiso 1 1 calc R . . C37 C 0.8429(6) 0.6786(3) 1.1888(7) 0.074(3) Uani 1 1 d . . . H37A H 0.8868 0.6991 1.1775 0.111 Uiso 1 1 calc R . . H37B H 0.8750 0.6652 1.2648 0.111 Uiso 1 1 calc R . . H37C H 0.7823 0.6915 1.1876 0.111 Uiso 1 1 calc R . . C38 C 0.9346(6) 0.6153(3) 1.0860(8) 0.086(3) Uani 1 1 d . . . H38A H 0.9263 0.5959 1.0224 0.129 Uiso 1 1 calc R . . H38B H 0.9590 0.6013 1.1621 0.129 Uiso 1 1 calc R . . H38C H 0.9816 0.6361 1.0845 0.129 Uiso 1 1 calc R . . C39 C 0.7364(5) 0.5993(2) 1.1014(7) 0.056(2) Uani 1 1 d . . . H39A H 0.6801 0.6119 1.1130 0.085 Uiso 1 1 calc R . . H39B H 0.7765 0.5853 1.1737 0.085 Uiso 1 1 calc R . . H39C H 0.7131 0.5799 1.0363 0.085 Uiso 1 1 calc R . . C40 C 0.7381(6) 0.5614(2) 0.8027(7) 0.068(2) Uani 1 1 d . . . H40A H 0.6995 0.5469 0.8422 0.081 Uiso 1 1 calc R . . H40B H 0.7971 0.5730 0.8636 0.081 Uiso 1 1 calc R . . C41 C 0.7663(8) 0.5332(3) 0.7226(9) 0.094(3) Uani 1 1 d . . . H41A H 0.8311 0.5209 0.7652 0.112 Uiso 1 1 calc R . . H41B H 0.7172 0.5115 0.6928 0.112 Uiso 1 1 calc R . . C42 C 0.7694(8) 0.5584(3) 0.6259(8) 0.098(4) Uani 1 1 d . . . H42A H 0.7525 0.5425 0.5524 0.118 Uiso 1 1 calc R . . H42B H 0.8354 0.5703 0.6448 0.118 Uiso 1 1 calc R . . C43 C 0.6943(6) 0.5909(3) 0.6135(7) 0.069(2) Uani 1 1 d . . . H43A H 0.7182 0.6171 0.5960 0.083 Uiso 1 1 calc R . . H43B H 0.6321 0.5842 0.5486 0.083 Uiso 1 1 calc R . . C44 C 0.1286(8) 0.6091(3) 0.5393(9) 0.087(3) Uiso 1 1 d . . . C45 C 0.1348(10) 0.5697(4) 0.4996(11) 0.122(4) Uiso 1 1 d . . . H45 H 0.1959 0.5574 0.5096 0.146 Uiso 1 1 calc R . . C46 C 0.0439(12) 0.5494(5) 0.4434(14) 0.161(6) Uiso 1 1 d . . . H46 H 0.0427 0.5228 0.4143 0.193 Uiso 1 1 calc R . . C47 C -0.0430(10) 0.5690(4) 0.4315(11) 0.122(4) Uiso 1 1 d D . . H47 H -0.1018 0.5546 0.3913 0.146 Uiso 1 1 calc R . . C48 C -0.0536(10) 0.6070(4) 0.4714(12) 0.143(5) Uiso 1 1 d D . . H48 H -0.1146 0.6187 0.4643 0.172 Uiso 1 1 calc R . . C49 C 0.0392(8) 0.6264(4) 0.5251(10) 0.107(4) Uiso 1 1 d D . . H49 H 0.0394 0.6532 0.5530 0.128 Uiso 1 1 calc R . . C50 C 0.2228(8) 0.6305(3) 0.6011(10) 0.101(3) Uiso 1 1 d . . . H50A H 0.2775 0.6117 0.6158 0.151 Uiso 1 1 calc R . . H50B H 0.2233 0.6412 0.6763 0.151 Uiso 1 1 calc R . . H50C H 0.2297 0.6528 0.5519 0.151 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 0.02595(14) 0.02600(14) 0.02764(14) 0.00098(11) 0.01151(10) 0.00260(11) Si1 0.0320(10) 0.0484(12) 0.0640(13) 0.0012(9) 0.0213(9) -0.0085(8) Si2 0.0300(9) 0.0471(11) 0.0541(12) 0.0070(9) 0.0064(9) 0.0038(8) O1 0.037(2) 0.029(2) 0.027(2) -0.0003(17) 0.0122(18) 0.0072(18) O2 0.036(2) 0.032(2) 0.034(2) -0.0030(17) 0.0207(19) -0.0013(18) O3 0.047(3) 0.045(3) 0.041(3) 0.004(2) 0.023(2) 0.018(2) N1 0.026(2) 0.024(2) 0.025(2) -0.0057(19) 0.004(2) -0.0042(19) N2 0.031(3) 0.030(3) 0.023(2) -0.0036(19) 0.011(2) -0.002(2) N3 0.024(3) 0.036(3) 0.048(3) -0.001(2) 0.016(2) -0.003(2) C1 0.030(3) 0.029(3) 0.026(3) 0.002(2) 0.013(3) 0.003(2) C2 0.037(3) 0.027(3) 0.030(3) 0.003(2) 0.019(3) 0.002(3) C3 0.039(3) 0.039(4) 0.021(3) 0.003(2) 0.010(3) 0.001(3) C4 0.026(3) 0.034(3) 0.033(3) 0.005(3) 0.014(3) 0.003(2) C5 0.032(3) 0.023(3) 0.035(3) 0.001(2) 0.018(3) 0.000(2) C6 0.028(3) 0.027(3) 0.029(3) -0.002(2) 0.012(3) 0.001(2) C7 0.028(3) 0.030(3) 0.028(3) 0.003(2) 0.009(3) 0.003(2) C8 0.042(3) 0.020(3) 0.025(3) 0.004(2) 0.012(3) 0.002(2) C9 0.039(4) 0.031(3) 0.036(3) 0.002(3) 0.016(3) -0.001(3) C10 0.031(3) 0.026(3) 0.039(3) 0.005(3) 0.016(3) 0.002(2) C11 0.034(3) 0.032(3) 0.028(3) 0.003(2) 0.012(3) 0.007(3) C12 0.034(3) 0.023(3) 0.024(3) 0.000(2) 0.012(3) 0.000(2) C13 0.041(3) 0.027(3) 0.028(3) -0.002(2) 0.011(3) 0.002(3) C14 0.028(3) 0.027(3) 0.027(3) 0.001(2) 0.008(2) 0.001(2) C15 0.036(3) 0.024(3) 0.031(3) -0.006(2) 0.007(3) -0.003(2) C16 0.037(3) 0.031(3) 0.027(3) -0.009(2) 0.007(3) -0.003(3) C17 0.043(4) 0.029(3) 0.029(3) 0.000(2) 0.017(3) -0.001(3) C18 0.059(4) 0.032(3) 0.026(3) -0.002(3) 0.018(3) 0.005(3) C19 0.084(6) 0.048(4) 0.032(4) -0.004(3) 0.019(4) 0.015(4) C20 0.065(5) 0.038(4) 0.045(4) 0.004(3) 0.034(4) 0.013(3) C21 0.069(5) 0.031(4) 0.037(4) 0.002(3) 0.016(3) 0.002(3) C22 0.025(3) 0.038(4) 0.042(4) 0.006(3) 0.009(3) 0.007(3) C23 0.028(4) 0.068(5) 0.085(6) 0.008(4) 0.019(4) -0.004(3) C24 0.058(5) 0.087(6) 0.041(4) 0.017(4) 0.015(4) 0.035(4) C25 0.035(4) 0.050(4) 0.067(5) -0.001(4) 0.009(4) 0.019(3) C26 0.060(4) 0.024(3) 0.037(3) 0.002(3) 0.030(3) 0.004(3) C27 0.090(6) 0.027(4) 0.080(6) -0.018(4) 0.057(5) -0.004(4) C28 0.071(5) 0.041(4) 0.053(4) 0.011(3) 0.036(4) 0.022(4) C29 0.068(5) 0.035(4) 0.040(4) -0.002(3) 0.030(4) 0.003(3) C30 0.035(3) 0.037(4) 0.055(4) 0.007(3) 0.017(3) 0.003(3) C34 0.060(5) 0.084(6) 0.080(6) 0.031(5) 0.033(5) -0.006(4) C35 0.057(5) 0.089(7) 0.110(8) 0.012(6) 0.051(5) 0.005(5) C36 0.103(7) 0.072(6) 0.100(7) -0.021(5) 0.051(6) -0.050(6) C37 0.072(6) 0.074(6) 0.052(5) -0.005(4) -0.008(4) -0.013(5) C38 0.047(5) 0.114(8) 0.087(7) 0.032(6) 0.013(5) 0.030(5) C39 0.056(5) 0.042(4) 0.061(5) 0.009(3) 0.008(4) 0.003(3) C40 0.084(6) 0.066(5) 0.070(5) 0.028(4) 0.048(5) 0.048(5) C41 0.116(8) 0.073(7) 0.106(8) 0.013(6) 0.057(7) 0.054(6) C42 0.114(8) 0.130(9) 0.063(6) 0.006(6) 0.047(6) 0.066(7) C43 0.073(6) 0.091(7) 0.055(5) 0.005(4) 0.036(4) 0.032(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 O2 2.125(4) . ? Yb1 O1 2.135(4) . ? Yb1 N3 2.245(5) . ? Yb1 O3 2.391(4) . ? Yb1 N2 2.499(4) . ? Yb1 N1 2.507(4) . ? Yb1 C14 2.771(6) . ? Yb1 Si1 3.3808(18) . ? Yb1 Si2 3.5025(19) . ? Si1 N3 1.716(5) . ? Si1 C34 1.863(8) . ? Si1 C35 1.869(8) . ? Si1 C36 1.875(8) . ? Si2 N3 1.726(5) . ? Si2 C38 1.873(8) . ? Si2 C39 1.876(7) . ? Si2 C37 1.895(8) . ? O1 C1 1.344(6) . ? O2 C7 1.335(6) . ? O3 C43 1.438(8) . ? O3 C40 1.445(8) . ? N1 C13 1.454(7) . ? N1 C14 1.457(7) . ? N1 C15 1.496(7) . ? N2 C17 1.459(7) . ? N2 C14 1.465(7) . ? N2 C16 1.477(7) . ? C1 C6 1.416(7) . ? C1 C2 1.425(8) . ? C2 C3 1.397(8) . ? C2 C18 1.533(8) . ? C3 C4 1.391(8) . ? C3 H3 0.9400 . ? C4 C5 1.387(8) . ? C4 C22 1.536(8) . ? C5 C6 1.385(8) . ? C5 H5 0.9400 . ? C6 C13 1.514(8) . ? C7 C12 1.408(8) . ? C7 C8 1.429(8) . ? C8 C9 1.387(8) . ? C8 C26 1.541(8) . ? C9 C10 1.399(8) . ? C9 H9 0.9400 . ? C10 C11 1.387(8) . ? C10 C30 1.537(8) . ? C11 C12 1.381(8) . ? C11 H11 0.9400 . ? C12 C17 1.506(8) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.533(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 C19 1.523(9) . ? C18 C21 1.530(8) . ? C18 C20 1.537(9) . ? 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 C25 1.521(9) . ? C22 C23 1.524(9) . ? C22 C24 1.526(9) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 C28 1.525(9) . ? C26 C29 1.526(8) . ? C26 C27 1.536(9) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 C32 1.525(16) . ? C30 C31' 1.53(3) . ? C30 C33 1.537(12) . ? C30 C31 1.539(15) . ? C30 C32' 1.543(17) . ? C30 C33' 1.55(3) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? 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 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C40 C41 1.496(11) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 C42 1.443(12) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 C43 1.492(11) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 C49 1.369(13) . ? C44 C45 1.393(15) . ? C44 C50 1.475(13) . ? C45 C46 1.411(17) . ? C45 H45 0.9400 . ? C46 C47 1.376(17) . ? C46 H46 0.9400 . ? C47 C48 1.365(13) . ? C47 H47 0.9400 . ? C48 C49 1.415(13) . ? C48 H48 0.9400 . ? C49 H49 0.9400 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C50 H50C 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 O2 Yb1 O1 108.44(15) . . ? O2 Yb1 N3 123.22(17) . . ? O1 Yb1 N3 125.81(17) . . ? O2 Yb1 O3 83.28(15) . . ? O1 Yb1 O3 86.21(14) . . ? N3 Yb1 O3 84.74(17) . . ? O2 Yb1 N2 74.35(14) . . ? O1 Yb1 N2 113.02(14) . . ? N3 Yb1 N2 96.51(16) . . ? O3 Yb1 N2 154.05(15) . . ? O2 Yb1 N1 117.96(14) . . ? O1 Yb1 N1 73.75(14) . . ? N3 Yb1 N1 93.93(16) . . ? O3 Yb1 N1 154.28(15) . . ? N2 Yb1 N1 51.65(15) . . ? O2 Yb1 C14 86.45(15) . . ? O1 Yb1 C14 81.39(15) . . ? N3 Yb1 C14 114.72(17) . . ? O3 Yb1 C14 160.52(16) . . ? N2 Yb1 C14 31.76(15) . . ? N1 Yb1 C14 31.53(15) . . ? O2 Yb1 Si1 146.91(11) . . ? O1 Yb1 Si1 98.85(11) . . ? N3 Yb1 Si1 26.98(13) . . ? O3 Yb1 Si1 80.18(12) . . ? N2 Yb1 Si1 112.01(11) . . ? N1 Yb1 Si1 87.04(11) . . ? C14 Yb1 Si1 116.47(12) . . ? O2 Yb1 Si2 99.67(11) . . ? O1 Yb1 Si2 150.04(11) . . ? N3 Yb1 Si2 24.33(13) . . ? O3 Yb1 Si2 87.00(11) . . ? N2 Yb1 Si2 84.03(11) . . ? N1 Yb1 Si2 102.26(10) . . ? C14 Yb1 Si2 111.09(12) . . ? Si1 Yb1 Si2 51.21(5) . . ? N3 Si1 C34 111.6(3) . . ? N3 Si1 C35 114.1(3) . . ? C34 Si1 C35 104.4(4) . . ? N3 Si1 C36 114.0(3) . . ? C34 Si1 C36 105.6(4) . . ? C35 Si1 C36 106.3(4) . . ? N3 Si1 Yb1 36.42(17) . . ? C34 Si1 Yb1 76.1(2) . . ? C35 Si1 Yb1 117.4(3) . . ? C36 Si1 Yb1 134.5(3) . . ? N3 Si2 C38 115.0(3) . . ? N3 Si2 C39 110.6(3) . . ? C38 Si2 C39 106.0(4) . . ? N3 Si2 C37 114.3(3) . . ? C38 Si2 C37 104.1(4) . . ? C39 Si2 C37 106.1(4) . . ? N3 Si2 Yb1 32.40(16) . . ? C38 Si2 Yb1 128.2(3) . . ? C39 Si2 Yb1 78.2(2) . . ? C37 Si2 Yb1 124.8(3) . . ? C1 O1 Yb1 144.0(3) . . ? C7 O2 Yb1 139.7(3) . . ? C43 O3 C40 108.7(5) . . ? C43 O3 Yb1 133.9(4) . . ? C40 O3 Yb1 117.0(4) . . ? C13 N1 C14 114.9(4) . . ? C13 N1 C15 112.1(4) . . ? C14 N1 C15 103.0(4) . . ? C13 N1 Yb1 126.0(3) . . ? C14 N1 Yb1 84.3(3) . . ? C15 N1 Yb1 111.2(3) . . ? C17 N2 C14 114.8(4) . . ? C17 N2 C16 113.0(4) . . ? C14 N2 C16 102.1(4) . . ? C17 N2 Yb1 124.7(3) . . ? C14 N2 Yb1 84.4(3) . . ? C16 N2 Yb1 112.2(3) . . ? Si1 N3 Si2 119.8(3) . . ? Si1 N3 Yb1 116.6(3) . . ? Si2 N3 Yb1 123.3(3) . . ? O1 C1 C6 120.8(5) . . ? O1 C1 C2 121.5(5) . . ? C6 C1 C2 117.8(5) . . ? C3 C2 C1 118.5(5) . . ? C3 C2 C18 119.7(5) . . ? C1 C2 C18 121.8(5) . . ? C4 C3 C2 123.9(5) . . ? C4 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? C5 C4 C3 116.3(5) . . ? C5 C4 C22 122.9(5) . . ? C3 C4 C22 120.8(5) . . ? C6 C5 C4 122.6(5) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C1 120.5(5) . . ? C5 C6 C13 116.5(5) . . ? C1 C6 C13 122.9(5) . . ? O2 C7 C12 121.0(5) . . ? O2 C7 C8 122.2(5) . . ? C12 C7 C8 116.8(5) . . ? C9 C8 C7 118.7(5) . . ? C9 C8 C26 120.4(5) . . ? C7 C8 C26 120.8(5) . . ? C8 C9 C10 124.2(6) . . ? C8 C9 H9 117.9 . . ? C10 C9 H9 117.9 . . ? C11 C10 C9 115.5(5) . . ? C11 C10 C30 121.6(5) . . ? C9 C10 C30 122.8(5) . . ? C12 C11 C10 122.6(5) . . ? C12 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? C11 C12 C7 121.3(5) . . ? C11 C12 C17 117.3(5) . . ? C7 C12 C17 121.2(5) . . ? N1 C13 C6 115.6(5) . . ? N1 C13 H13A 108.4 . . ? C6 C13 H13A 108.4 . . ? N1 C13 H13B 108.4 . . ? C6 C13 H13B 108.4 . . ? H13A C13 H13B 107.4 . . ? N1 C14 N2 96.5(4) . . ? N1 C14 Yb1 64.2(3) . . ? N2 C14 Yb1 63.8(3) . . ? N1 C14 H14A 112.4 . . ? N2 C14 H14A 112.4 . . ? Yb1 C14 H14A 76.2 . . ? N1 C14 H14B 112.4 . . ? N2 C14 H14B 112.4 . . ? Yb1 C14 H14B 173.8 . . ? H14A C14 H14B 110.0 . . ? N1 C15 C16 101.7(4) . . ? N1 C15 H15A 111.4 . . ? C16 C15 H15A 111.4 . . ? N1 C15 H15B 111.4 . . ? C16 C15 H15B 111.4 . . ? H15A C15 H15B 109.3 . . ? N2 C16 C15 103.4(4) . . ? N2 C16 H16A 111.1 . . ? C15 C16 H16A 111.1 . . ? N2 C16 H16B 111.1 . . ? C15 C16 H16B 111.1 . . ? H16A C16 H16B 109.0 . . ? N2 C17 C12 115.7(5) . . ? N2 C17 H17A 108.4 . . ? C12 C17 H17A 108.4 . . ? N2 C17 H17B 108.4 . . ? C12 C17 H17B 108.4 . . ? H17A C17 H17B 107.4 . . ? C19 C18 C21 106.6(5) . . ? C19 C18 C2 112.8(5) . . ? C21 C18 C2 110.3(5) . . ? C19 C18 C20 107.5(5) . . ? C21 C18 C20 111.2(5) . . ? C2 C18 C20 108.4(5) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C25 C22 C23 109.3(6) . . ? C25 C22 C24 107.4(6) . . ? C23 C22 C24 108.9(6) . . ? C25 C22 C4 112.4(5) . . ? C23 C22 C4 107.8(5) . . ? C24 C22 C4 111.1(5) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C28 C26 C29 111.0(5) . . ? C28 C26 C27 107.0(5) . . ? C29 C26 C27 106.7(5) . . ? C28 C26 C8 108.4(5) . . ? C29 C26 C8 111.6(5) . . ? C27 C26 C8 112.1(5) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C30 C31' 134.7(13) . . ? C32 C30 C10 109.0(7) . . ? C31' C30 C10 109.9(11) . . ? C32 C30 C33 108.3(9) . . ? C31' C30 C33 77.6(13) . . ? C10 C30 C33 111.6(7) . . ? C32 C30 C31 109.7(9) . . ? C31' C30 C31 33.6(11) . . ? C10 C30 C31 110.2(7) . . ? C33 C30 C31 108.0(9) . . ? C32 C30 C32' 41.5(11) . . ? C31' C30 C32' 102.0(16) . . ? C10 C30 C32' 110.8(12) . . ? C33 C30 C32' 134.7(13) . . ? C31 C30 C32' 70.6(13) . . ? C32 C30 C33' 58.9(11) . . ? C31' C30 C33' 122.6(15) . . ? C10 C30 C33' 112.5(11) . . ? C33 C30 C33' 51.8(11) . . ? C31 C30 C33' 137.2(12) . . ? C32' C30 C33' 97.2(16) . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si2 C37 H37A 109.5 . . ? Si2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si2 C38 H38A 109.5 . . ? Si2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si2 C39 H39A 109.5 . . ? Si2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O3 C40 C41 104.9(6) . . ? O3 C40 H40A 110.8 . . ? C41 C40 H40A 110.8 . . ? O3 C40 H40B 110.8 . . ? C41 C40 H40B 110.8 . . ? H40A C40 H40B 108.8 . . ? C42 C41 C40 105.4(7) . . ? C42 C41 H41A 110.7 . . ? C40 C41 H41A 110.7 . . ? C42 C41 H41B 110.7 . . ? C40 C41 H41B 110.7 . . ? H41A C41 H41B 108.8 . . ? C41 C42 C43 104.6(7) . . ? C41 C42 H42A 110.8 . . ? C43 C42 H42A 110.8 . . ? C41 C42 H42B 110.8 . . ? C43 C42 H42B 110.8 . . ? H42A C42 H42B 108.9 . . ? O3 C43 C42 107.0(6) . . ? O3 C43 H43A 110.3 . . ? C42 C43 H43A 110.3 . . ? O3 C43 H43B 110.3 . . ? C42 C43 H43B 110.3 . . ? H43A C43 H43B 108.6 . . ? C49 C44 C45 121.3(11) . . ? C49 C44 C50 121.8(10) . . ? C45 C44 C50 116.9(11) . . ? C44 C45 C46 115.9(13) . . ? C44 C45 H45 122.1 . . ? C46 C45 H45 122.1 . . ? C47 C46 C45 119.4(16) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C48 C47 C46 127.3(15) . . ? C48 C47 H47 116.3 . . ? C46 C47 H47 116.3 . . ? C47 C48 C49 111.3(13) . . ? C47 C48 H48 124.4 . . ? C49 C48 H48 124.4 . . ? C44 C49 C48 124.8(12) . . ? C44 C49 H49 117.6 . . ? C48 C49 H49 117.6 . . ? C44 C50 H50A 109.5 . . ? C44 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C44 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.609 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.105 #===================================================end data_complex6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H76 N3 O3 Si2 Y' _chemical_formula_sum 'C43 H76 N3 O3 Si2 Y' _chemical_formula_weight 828.16 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 12.5254(16) _cell_length_b 10.5775(13) _cell_length_c 35.864(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.665(4) _cell_angle_gamma 90.00 _cell_volume 4751.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16940 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.158 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 1.315 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.258 _exptl_absorpt_correction_T_max 0.674 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22329 _diffrn_reflns_av_R_equivalents 0.0905 _diffrn_reflns_av_sigmaI/netI 0.1367 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8665 _reflns_number_gt 5688 _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 ? _computing_publication_material ? _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^)+(0.0684P)^2^+5.8038P] 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 8665 _refine_ls_number_parameters 449 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1616 _refine_ls_R_factor_gt 0.1034 _refine_ls_wR_factor_ref 0.2069 _refine_ls_wR_factor_gt 0.1846 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.157 _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 0.78501(5) 0.53369(6) 0.393966(18) 0.0323(2) Uani 1 1 d . . . Si1 Si 0.76310(16) 0.32296(19) 0.47033(6) 0.0435(5) Uani 1 1 d . . . Si2 Si 0.59171(15) 0.31544(19) 0.41190(6) 0.0461(6) Uani 1 1 d . . . O1 O 0.9487(3) 0.5723(4) 0.40524(13) 0.0391(11) Uani 1 1 d . . . O2 O 0.7526(3) 0.6315(4) 0.34269(13) 0.0427(12) Uani 1 1 d . . . O3 O 0.8416(4) 0.3576(4) 0.35545(14) 0.0508(13) Uani 1 1 d . . . N1 N 0.7852(4) 0.7144(5) 0.44102(15) 0.0341(13) Uani 1 1 d . . . N2 N 0.6434(4) 0.7009(5) 0.40551(16) 0.0393(14) Uani 1 1 d . . . N3 N 0.7064(4) 0.3795(5) 0.42984(15) 0.0357(13) Uani 1 1 d . . . C1 C 1.0126(5) 0.6743(6) 0.40943(19) 0.0340(16) Uani 1 1 d . . . C2 C 1.1138(5) 0.6793(6) 0.39272(19) 0.0391(17) Uani 1 1 d . . . C3 C 1.1706(5) 0.7910(6) 0.3952(2) 0.0447(19) Uani 1 1 d . . . H3 H 1.2366 0.7946 0.3837 0.054 Uiso 1 1 calc R . . C4 C 1.1359(5) 0.8983(7) 0.4138(2) 0.0414(18) Uani 1 1 d . . . C5 C 1.0391(5) 0.8883(6) 0.4321(2) 0.0419(18) Uani 1 1 d . . . H5 H 1.0137 0.9571 0.4455 0.050 Uiso 1 1 calc R . . C6 C 0.9791(5) 0.7769(6) 0.43076(18) 0.0342(16) Uani 1 1 d . . . C7 C 0.7009(5) 0.7276(6) 0.3252(2) 0.0407(18) Uani 1 1 d . . . C8 C 0.7411(6) 0.7817(7) 0.2921(2) 0.0468(19) Uani 1 1 d . . . C9 C 0.6786(6) 0.8732(7) 0.2743(2) 0.054(2) Uani 1 1 d . . . H9 H 0.7031 0.9063 0.2520 0.064 Uiso 1 1 calc R . . C10 C 0.5821(6) 0.9181(7) 0.2877(2) 0.053(2) Uani 1 1 d . . . C11 C 0.5513(6) 0.8716(7) 0.3218(2) 0.050(2) Uani 1 1 d . . . H11 H 0.4902 0.9045 0.3326 0.060 Uiso 1 1 calc R . . C12 C 0.6071(5) 0.7780(6) 0.3408(2) 0.0391(17) Uani 1 1 d . . . C13 C 0.8845(5) 0.7681(7) 0.4569(2) 0.0448(19) Uani 1 1 d . . . H13A H 0.9056 0.7172 0.4782 0.054 Uiso 1 1 calc R . . H13B H 0.8689 0.8523 0.4660 0.054 Uiso 1 1 calc R . . C14 C 0.7328(5) 0.7887(6) 0.4121(2) 0.0376(17) Uani 1 1 d . . . H14A H 0.7768 0.7993 0.3903 0.045 Uiso 1 1 calc R . . H14B H 0.7092 0.8704 0.4211 0.045 Uiso 1 1 calc R . . C15 C 0.6998(5) 0.6989(7) 0.4686(2) 0.0470(19) Uani 1 1 d . . . H15A H 0.6949 0.7719 0.4848 0.056 Uiso 1 1 calc R . . H15B H 0.7106 0.6236 0.4836 0.056 Uiso 1 1 calc R . . C16 C 0.6001(5) 0.6866(7) 0.4433(2) 0.050(2) Uani 1 1 d . . . H16A H 0.5663 0.6048 0.4463 0.059 Uiso 1 1 calc R . . H16B H 0.5486 0.7525 0.4486 0.059 Uiso 1 1 calc R . . C17 C 0.5625(5) 0.7388(8) 0.3776(2) 0.050(2) Uani 1 1 d . . . H17A H 0.5216 0.8086 0.3876 0.061 Uiso 1 1 calc R . . H17B H 0.5138 0.6687 0.3736 0.061 Uiso 1 1 calc R . . C18 C 1.1630(5) 0.5627(7) 0.3744(2) 0.048(2) Uani 1 1 d . . . C19 C 1.2790(6) 0.5858(9) 0.3620(3) 0.083(3) Uani 1 1 d . . . H19A H 1.3216 0.6117 0.3831 0.125 Uiso 1 1 calc R . . H19B H 1.2799 0.6508 0.3433 0.125 Uiso 1 1 calc R . . H19C H 1.3077 0.5091 0.3518 0.125 Uiso 1 1 calc R . . C20 C 1.0993(6) 0.5211(8) 0.3402(2) 0.065(2) Uani 1 1 d . . . H20A H 1.1269 0.4421 0.3312 0.098 Uiso 1 1 calc R . . H20B H 1.1052 0.5840 0.3210 0.098 Uiso 1 1 calc R . . H20C H 1.0256 0.5108 0.3466 0.098 Uiso 1 1 calc R . . C21 C 1.1686(6) 0.4560(7) 0.4028(2) 0.062(2) Uani 1 1 d . . . H21A H 1.0981 0.4369 0.4114 0.093 Uiso 1 1 calc R . . H21B H 1.2126 0.4815 0.4236 0.093 Uiso 1 1 calc R . . H21C H 1.1988 0.3822 0.3914 0.093 Uiso 1 1 calc R . . C22 C 1.2036(6) 1.0186(7) 0.4146(2) 0.052(2) Uani 1 1 d . . . C23 C 1.1557(7) 1.1222(7) 0.4384(3) 0.074(3) Uani 1 1 d . . . H23A H 1.0875 1.1463 0.4282 0.111 Uiso 1 1 calc R . . H23B H 1.2025 1.1942 0.4387 0.111 Uiso 1 1 calc R . . H23C H 1.1468 1.0918 0.4634 0.111 Uiso 1 1 calc R . . C24 C 1.2215(9) 1.0673(8) 0.3755(3) 0.091(3) Uani 1 1 d . . . H24A H 1.2568 1.0036 0.3611 0.137 Uiso 1 1 calc R . . H24B H 1.2651 1.1419 0.3765 0.137 Uiso 1 1 calc R . . H24C H 1.1540 1.0873 0.3640 0.137 Uiso 1 1 calc R . . C25 C 1.3133(7) 0.9887(8) 0.4328(3) 0.092(3) Uani 1 1 d . . . H25A H 1.3032 0.9604 0.4580 0.137 Uiso 1 1 calc R . . H25B H 1.3566 1.0636 0.4330 0.137 Uiso 1 1 calc R . . H25C H 1.3482 0.9237 0.4188 0.137 Uiso 1 1 calc R . . C26 C 0.8539(7) 0.7523(8) 0.2779(2) 0.063(2) Uani 1 1 d . . . C27 C 0.8799(7) 0.8244(9) 0.2431(3) 0.0889(18) Uani 1 1 d . . . H27A H 0.9530 0.8094 0.2366 0.133 Uiso 1 1 calc R . . H27B H 0.8693 0.9131 0.2473 0.133 Uiso 1 1 calc R . . H27C H 0.8341 0.7967 0.2230 0.133 Uiso 1 1 calc R . . C28 C 0.8670(7) 0.6111(10) 0.2698(3) 0.0889(18) Uani 1 1 d . . . H28A H 0.8198 0.5871 0.2498 0.133 Uiso 1 1 calc R . . H28B H 0.8502 0.5633 0.2917 0.133 Uiso 1 1 calc R . . H28C H 0.9395 0.5944 0.2629 0.133 Uiso 1 1 calc R . . C29 C 0.9342(7) 0.7918(10) 0.3083(3) 0.0889(18) Uani 1 1 d . . . H29A H 1.0054 0.7764 0.2998 0.133 Uiso 1 1 calc R . . H29B H 0.9217 0.7436 0.3305 0.133 Uiso 1 1 calc R . . H29C H 0.9257 0.8802 0.3136 0.133 Uiso 1 1 calc R . . C30 C 0.5139(7) 1.0182(8) 0.2660(2) 0.075(3) Uani 1 1 d D . . C31 C 0.4526(14) 1.1046(17) 0.2931(5) 0.068(4) Uiso 0.50 1 d PD . . C31' C 0.4991(15) 1.1343(15) 0.2905(5) 0.068(4) Uiso 0.50 1 d PD . . C32 C 0.4057(13) 0.9536(18) 0.2580(6) 0.079(4) Uiso 0.50 1 d PD . . C32' C 0.4446(15) 0.9599(18) 0.2365(5) 0.079(4) Uiso 0.50 1 d PD . . C33 C 0.5559(18) 1.051(2) 0.2275(5) 0.099(5) Uiso 0.50 1 d PD . . C33' C 0.5901(16) 1.102(2) 0.2433(6) 0.099(5) Uiso 0.50 1 d PD . . C34 C 0.6755(7) 0.3370(9) 0.5115(2) 0.075(3) Uani 1 1 d . . . H34A H 0.6512 0.4227 0.5138 0.113 Uiso 1 1 calc R . . H34B H 0.7149 0.3137 0.5336 0.113 Uiso 1 1 calc R . . H34C H 0.6151 0.2819 0.5085 0.113 Uiso 1 1 calc R . . C35 C 0.8876(6) 0.4090(9) 0.4828(3) 0.077(3) Uani 1 1 d . . . H35A H 0.9378 0.4009 0.4629 0.116 Uiso 1 1 calc R . . H35B H 0.9178 0.3739 0.5052 0.116 Uiso 1 1 calc R . . H35C H 0.8717 0.4968 0.4866 0.116 Uiso 1 1 calc R . . C36 C 0.8034(8) 0.1522(8) 0.4688(3) 0.080(3) Uani 1 1 d . . . H36A H 0.7414 0.1007 0.4645 0.120 Uiso 1 1 calc R . . H36B H 0.8362 0.1290 0.4922 0.120 Uiso 1 1 calc R . . H36C H 0.8533 0.1395 0.4490 0.120 Uiso 1 1 calc R . . C37 C 0.4704(6) 0.3392(9) 0.4412(3) 0.088(3) Uani 1 1 d . . . H37A H 0.4696 0.2773 0.4608 0.131 Uiso 1 1 calc R . . H37B H 0.4074 0.3301 0.4259 0.131 Uiso 1 1 calc R . . H37C H 0.4720 0.4224 0.4519 0.131 Uiso 1 1 calc R . . C38 C 0.5967(7) 0.1419(7) 0.4028(3) 0.078(3) Uani 1 1 d . . . H38A H 0.6595 0.1222 0.3889 0.118 Uiso 1 1 calc R . . H38B H 0.5344 0.1169 0.3888 0.118 Uiso 1 1 calc R . . H38C H 0.5987 0.0972 0.4261 0.118 Uiso 1 1 calc R . . C39 C 0.5598(7) 0.3894(9) 0.3657(3) 0.080(3) Uani 1 1 d . . . H39A H 0.5390 0.4759 0.3694 0.120 Uiso 1 1 calc R . . H39B H 0.5023 0.3440 0.3539 0.120 Uiso 1 1 calc R . . H39C H 0.6216 0.3863 0.3502 0.120 Uiso 1 1 calc R . . C40 C 0.9076(9) 0.2627(9) 0.3722(3) 0.1015(18) Uani 1 1 d D . . H40A H 0.8822 0.2432 0.3970 0.122 Uiso 1 1 calc R . . H40B H 0.9805 0.2930 0.3744 0.122 Uiso 1 1 calc R . . C41 C 0.9040(9) 0.1484(9) 0.3488(3) 0.1015(18) Uani 1 1 d D . . H41A H 0.8745 0.0779 0.3625 0.122 Uiso 1 1 calc R . . H41B H 0.9751 0.1259 0.3406 0.122 Uiso 1 1 calc R . . C42 C 0.8341(9) 0.1805(9) 0.3160(3) 0.1015(18) Uani 1 1 d D . . H42A H 0.8683 0.1570 0.2929 0.122 Uiso 1 1 calc R . . H42B H 0.7663 0.1367 0.3176 0.122 Uiso 1 1 calc R . . C43 C 0.8185(9) 0.3185(9) 0.3179(3) 0.1015(18) Uani 1 1 d D . . H43A H 0.8659 0.3608 0.3007 0.122 Uiso 1 1 calc R . . H43B H 0.7455 0.3399 0.3112 0.122 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 0.0323(3) 0.0278(3) 0.0370(4) 0.0014(3) 0.0028(3) -0.0002(3) Si1 0.0446(11) 0.0399(11) 0.0460(14) 0.0105(10) 0.0003(10) -0.0017(10) Si2 0.0352(11) 0.0363(11) 0.0666(16) 0.0009(10) -0.0018(10) -0.0054(10) O1 0.033(2) 0.033(2) 0.051(3) -0.008(2) 0.005(2) -0.001(2) O2 0.049(3) 0.035(3) 0.044(3) 0.009(2) 0.007(2) 0.007(2) O3 0.068(3) 0.040(3) 0.045(3) -0.009(2) 0.001(3) 0.009(3) N1 0.031(3) 0.033(3) 0.038(4) 0.000(3) 0.007(3) -0.004(3) N2 0.035(3) 0.039(3) 0.044(4) 0.002(3) 0.008(3) -0.002(3) N3 0.031(3) 0.032(3) 0.044(4) 0.004(3) 0.004(3) 0.000(3) C1 0.034(4) 0.026(3) 0.042(5) -0.004(3) -0.001(3) -0.008(3) C2 0.036(4) 0.039(4) 0.042(5) 0.001(3) 0.001(3) 0.004(3) C3 0.032(4) 0.045(4) 0.058(5) 0.000(4) 0.006(3) -0.002(4) C4 0.041(4) 0.040(4) 0.043(5) 0.000(3) 0.001(3) -0.006(4) C5 0.048(4) 0.032(4) 0.045(5) -0.002(3) -0.006(4) 0.002(4) C6 0.036(4) 0.035(4) 0.032(4) -0.006(3) 0.002(3) -0.005(3) C7 0.041(4) 0.035(4) 0.046(5) 0.002(3) -0.010(3) 0.003(3) C8 0.051(4) 0.050(5) 0.039(5) 0.006(4) -0.004(4) 0.001(4) C9 0.072(6) 0.039(4) 0.049(5) 0.012(4) -0.014(4) -0.002(4) C10 0.067(5) 0.042(4) 0.048(6) -0.008(4) -0.027(4) 0.012(4) C11 0.039(4) 0.051(5) 0.060(6) -0.009(4) -0.013(4) 0.008(4) C12 0.031(4) 0.041(4) 0.046(5) 0.002(3) -0.008(3) 0.003(3) C13 0.042(4) 0.040(4) 0.052(5) -0.009(4) 0.007(4) -0.003(4) C14 0.031(4) 0.034(4) 0.048(5) 0.000(3) 0.008(3) -0.001(3) C15 0.040(4) 0.051(5) 0.051(5) 0.000(4) 0.016(4) 0.002(4) C16 0.038(4) 0.049(5) 0.062(6) -0.005(4) 0.016(4) -0.001(4) C17 0.033(4) 0.065(5) 0.053(6) 0.005(4) -0.002(4) 0.012(4) C18 0.035(4) 0.050(5) 0.060(5) -0.016(4) 0.012(4) 0.002(4) C19 0.049(5) 0.072(6) 0.129(9) -0.021(6) 0.036(5) 0.005(5) C20 0.071(5) 0.068(6) 0.057(6) -0.020(5) 0.006(4) 0.020(5) C21 0.046(4) 0.048(5) 0.091(7) -0.009(5) -0.003(4) 0.013(4) C22 0.055(5) 0.042(4) 0.061(6) 0.010(4) 0.003(4) -0.008(4) C23 0.090(7) 0.037(4) 0.094(8) -0.008(5) 0.014(6) -0.022(5) C24 0.128(9) 0.059(6) 0.087(8) 0.014(5) 0.035(7) -0.029(6) C25 0.061(6) 0.057(6) 0.155(11) 0.009(6) -0.017(6) -0.018(5) C26 0.077(6) 0.057(5) 0.055(6) 0.030(4) 0.010(5) 0.004(5) C27 0.080(4) 0.104(5) 0.083(5) 0.020(4) 0.020(3) 0.011(4) C28 0.080(4) 0.104(5) 0.083(5) 0.020(4) 0.020(3) 0.011(4) C29 0.080(4) 0.104(5) 0.083(5) 0.020(4) 0.020(3) 0.011(4) C30 0.091(7) 0.062(5) 0.070(7) -0.009(5) -0.037(5) 0.022(5) C34 0.087(7) 0.082(6) 0.057(6) 0.004(5) 0.017(5) 0.006(6) C35 0.059(5) 0.090(7) 0.082(7) 0.031(6) -0.025(5) -0.016(5) C36 0.105(7) 0.058(5) 0.077(7) 0.023(5) 0.000(6) 0.022(5) C37 0.042(5) 0.099(8) 0.122(9) -0.018(7) 0.015(5) -0.024(5) C38 0.067(6) 0.049(5) 0.119(9) -0.004(5) -0.018(6) -0.010(5) C39 0.068(6) 0.085(7) 0.086(8) 0.014(6) -0.034(5) -0.017(5) C40 0.130(5) 0.075(3) 0.100(5) -0.027(3) -0.016(3) 0.028(4) C41 0.130(5) 0.075(3) 0.100(5) -0.027(3) -0.016(3) 0.028(4) C42 0.130(5) 0.075(3) 0.100(5) -0.027(3) -0.016(3) 0.028(4) C43 0.130(5) 0.075(3) 0.100(5) -0.027(3) -0.016(3) 0.028(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O1 2.125(4) . ? Y1 O2 2.145(4) . ? Y1 N3 2.305(5) . ? Y1 O3 2.429(5) . ? Y1 N2 2.542(5) . ? Y1 N1 2.549(5) . ? Y1 C14 2.852(6) . ? Y1 Si2 3.412(2) . ? Si1 N3 1.716(6) . ? Si1 C35 1.856(8) . ? Si1 C34 1.857(8) . ? Si1 C36 1.877(8) . ? Si2 N3 1.708(5) . ? Si2 C38 1.866(8) . ? Si2 C39 1.871(9) . ? Si2 C37 1.874(8) . ? O1 C1 1.351(7) . ? O2 C7 1.355(7) . ? O3 C40 1.429(10) . ? O3 C43 1.434(11) . ? N1 C14 1.452(8) . ? N1 C15 1.475(8) . ? N1 C13 1.476(8) . ? N2 C17 1.471(8) . ? N2 C14 1.472(8) . ? N2 C16 1.472(9) . ? C1 C6 1.395(9) . ? C1 C2 1.409(9) . ? C2 C3 1.382(9) . ? C2 C18 1.530(9) . ? C3 C4 1.389(9) . ? C3 H3 0.9300 . ? C4 C5 1.389(9) . ? C4 C22 1.529(10) . ? C5 C6 1.398(9) . ? C5 H5 0.9300 . ? C6 C13 1.523(9) . ? C7 C12 1.411(9) . ? C7 C8 1.415(10) . ? C8 C9 1.396(9) . ? C8 C26 1.539(11) . ? C9 C10 1.389(11) . ? C9 H9 0.9300 . ? C10 C11 1.377(11) . ? C10 C30 1.562(10) . ? C11 C12 1.385(9) . ? C11 H11 0.9300 . ? C12 C17 1.500(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.541(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C21 1.521(11) . ? C18 C20 1.522(10) . ? C18 C19 1.545(9) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C24 1.516(11) . ? C22 C23 1.517(11) . ? C22 C25 1.546(11) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.503(11) . ? C26 C28 1.531(12) . ? C26 C29 1.532(12) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C32' 1.494(15) . ? C30 C33 1.523(16) . ? C30 C31' 1.523(15) . ? C30 C33' 1.539(16) . ? C30 C32 1.542(15) . ? C30 C31 1.546(15) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.472(10) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.494(11) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.475(10) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 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 Y1 O2 104.08(17) . . ? O1 Y1 N3 116.56(18) . . ? O2 Y1 N3 137.90(18) . . ? O1 Y1 O3 88.18(16) . . ? O2 Y1 O3 86.31(17) . . ? N3 Y1 O3 84.51(18) . . ? O1 Y1 N2 120.60(17) . . ? O2 Y1 N2 71.25(17) . . ? N3 Y1 N2 95.62(17) . . ? O3 Y1 N2 146.58(18) . . ? O1 Y1 N1 74.71(16) . . ? O2 Y1 N1 101.82(17) . . ? N3 Y1 N1 99.10(18) . . ? O3 Y1 N1 162.35(17) . . ? N2 Y1 N1 50.67(17) . . ? O1 Y1 C14 89.90(17) . . ? O2 Y1 C14 72.42(18) . . ? N3 Y1 C14 116.17(19) . . ? O3 Y1 C14 157.49(19) . . ? N2 Y1 C14 30.99(17) . . ? N1 Y1 C14 30.53(17) . . ? O1 Y1 Si2 141.21(13) . . ? O2 Y1 Si2 111.11(13) . . ? N3 Y1 Si2 26.81(13) . . ? O3 Y1 Si2 78.52(12) . . ? N2 Y1 Si2 86.67(12) . . ? N1 Y1 Si2 112.19(12) . . ? C14 Y1 Si2 115.57(13) . . ? N3 Si1 C35 111.8(3) . . ? N3 Si1 C34 113.8(3) . . ? C35 Si1 C34 105.8(4) . . ? N3 Si1 C36 114.8(4) . . ? C35 Si1 C36 104.7(4) . . ? C34 Si1 C36 105.2(4) . . ? N3 Si2 C38 115.2(3) . . ? N3 Si2 C39 109.8(3) . . ? C38 Si2 C39 105.3(4) . . ? N3 Si2 C37 114.8(4) . . ? C38 Si2 C37 105.0(4) . . ? C39 Si2 C37 105.9(4) . . ? N3 Si2 Y1 37.51(18) . . ? C38 Si2 Y1 127.4(3) . . ? C39 Si2 Y1 72.2(3) . . ? C37 Si2 Y1 126.6(3) . . ? C1 O1 Y1 138.1(4) . . ? C7 O2 Y1 147.5(4) . . ? C40 O3 C43 107.5(6) . . ? C40 O3 Y1 118.1(5) . . ? C43 O3 Y1 134.2(5) . . ? C14 N1 C15 102.3(5) . . ? C14 N1 C13 116.1(5) . . ? C15 N1 C13 113.5(5) . . ? C14 N1 Y1 86.3(4) . . ? C15 N1 Y1 111.4(4) . . ? C13 N1 Y1 122.6(4) . . ? C17 N2 C14 117.0(5) . . ? C17 N2 C16 113.3(5) . . ? C14 N2 C16 101.8(5) . . ? C17 N2 Y1 123.8(4) . . ? C14 N2 Y1 86.2(3) . . ? C16 N2 Y1 110.1(4) . . ? Si2 N3 Si1 121.2(3) . . ? Si2 N3 Y1 115.7(3) . . ? Si1 N3 Y1 122.9(3) . . ? O1 C1 C6 120.1(6) . . ? O1 C1 C2 121.1(6) . . ? C6 C1 C2 118.8(6) . . ? C3 C2 C1 118.0(6) . . ? C3 C2 C18 120.5(6) . . ? C1 C2 C18 121.4(6) . . ? C2 C3 C4 124.5(6) . . ? C2 C3 H3 117.8 . . ? C4 C3 H3 117.8 . . ? C3 C4 C5 116.4(6) . . ? C3 C4 C22 120.8(6) . . ? C5 C4 C22 122.7(7) . . ? C4 C5 C6 121.3(7) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C1 C6 C5 120.6(6) . . ? C1 C6 C13 122.1(6) . . ? C5 C6 C13 116.9(6) . . ? O2 C7 C12 119.8(6) . . ? O2 C7 C8 121.2(6) . . ? C12 C7 C8 119.0(6) . . ? C9 C8 C7 117.5(7) . . ? C9 C8 C26 120.0(7) . . ? C7 C8 C26 122.2(6) . . ? C10 C9 C8 124.3(8) . . ? C10 C9 H9 117.8 . . ? C8 C9 H9 117.8 . . ? C11 C10 C9 116.0(7) . . ? C11 C10 C30 121.8(8) . . ? C9 C10 C30 122.1(8) . . ? C10 C11 C12 123.1(7) . . ? C10 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C11 C12 C7 119.6(7) . . ? C11 C12 C17 116.1(6) . . ? C7 C12 C17 124.3(6) . . ? N1 C13 C6 116.4(6) . . ? N1 C13 H13A 108.2 . . ? C6 C13 H13A 108.2 . . ? N1 C13 H13B 108.2 . . ? C6 C13 H13B 108.2 . . ? H13A C13 H13B 107.3 . . ? N1 C14 N2 96.3(5) . . ? N1 C14 Y1 63.1(3) . . ? N2 C14 Y1 62.8(3) . . ? N1 C14 H14A 112.5 . . ? N2 C14 H14A 112.5 . . ? Y1 C14 H14A 78.0 . . ? N1 C14 H14B 112.5 . . ? N2 C14 H14B 112.5 . . ? Y1 C14 H14B 172.0 . . ? H14A C14 H14B 110.0 . . ? N1 C15 C16 101.7(6) . . ? N1 C15 H15A 111.4 . . ? C16 C15 H15A 111.4 . . ? N1 C15 H15B 111.4 . . ? C16 C15 H15B 111.4 . . ? H15A C15 H15B 109.3 . . ? N2 C16 C15 103.3(5) . . ? N2 C16 H16A 111.1 . . ? C15 C16 H16A 111.1 . . ? N2 C16 H16B 111.1 . . ? C15 C16 H16B 111.1 . . ? H16A C16 H16B 109.1 . . ? N2 C17 C12 114.5(5) . . ? N2 C17 H17A 108.6 . . ? C12 C17 H17A 108.6 . . ? N2 C17 H17B 108.6 . . ? C12 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? C21 C18 C20 110.2(6) . . ? C21 C18 C2 109.1(6) . . ? C20 C18 C2 111.7(6) . . ? C21 C18 C19 105.9(7) . . ? C20 C18 C19 107.4(7) . . ? C2 C18 C19 112.4(6) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C23 109.8(7) . . ? C24 C22 C4 110.7(7) . . ? C23 C22 C4 112.9(6) . . ? C24 C22 C25 108.7(7) . . ? C23 C22 C25 105.4(7) . . ? C4 C22 C25 109.2(6) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C28 108.2(8) . . ? C27 C26 C29 107.8(8) . . ? C28 C26 C29 109.2(7) . . ? C27 C26 C8 112.5(7) . . ? C28 C26 C8 111.2(7) . . ? C29 C26 C8 107.9(7) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32' C30 C33 69.9(12) . . ? C32' C30 C31' 131.9(12) . . ? C33 C30 C31' 112.6(13) . . ? C32' C30 C33' 102.7(13) . . ? C33 C30 C33' 33.5(11) . . ? C31' C30 C33' 85.7(12) . . ? C32' C30 C32 35.2(9) . . ? C33 C30 C32 104.2(13) . . ? C31' C30 C32 110.6(12) . . ? C33' C30 C32 134.7(13) . . ? C32' C30 C31 113.6(12) . . ? C33 C30 C31 127.9(13) . . ? C31' C30 C31 25.2(9) . . ? C33' C30 C31 108.1(13) . . ? C32 C30 C31 86.4(11) . . ? C32' C30 C10 112.5(10) . . ? C33 C30 C10 114.4(11) . . ? C31' C30 C10 109.2(9) . . ? C33' C30 C10 108.3(11) . . ? C32 C30 C10 105.4(10) . . ? C31 C30 C10 111.1(10) . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si2 C37 H37A 109.5 . . ? Si2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si2 C38 H38A 109.5 . . ? Si2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si2 C39 H39A 109.5 . . ? Si2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O3 C40 C41 108.9(8) . . ? O3 C40 H40A 109.9 . . ? C41 C40 H40A 109.9 . . ? O3 C40 H40B 109.9 . . ? C41 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? C40 C41 C42 106.0(8) . . ? C40 C41 H41A 110.5 . . ? C42 C41 H41A 110.5 . . ? C40 C41 H41B 110.5 . . ? C42 C41 H41B 110.5 . . ? H41A C41 H41B 108.7 . . ? C43 C42 C41 105.4(8) . . ? C43 C42 H42A 110.7 . . ? C41 C42 H42A 110.7 . . ? C43 C42 H42B 110.7 . . ? C41 C42 H42B 110.7 . . ? H42A C42 H42B 108.8 . . ? O3 C43 C42 107.6(8) . . ? O3 C43 H43A 110.2 . . ? C42 C43 H43A 110.2 . . ? O3 C43 H43B 110.2 . . ? C42 C43 H43B 110.2 . . ? H43A C43 H43B 108.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.602 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.080 #===================================================end of CIF