# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_4c' _database_code_depnum_ccdc_archive 'CCDC 896985' #TrackingRef 'CCDC-896985.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H72 Cl Er Li2 N6 O' _chemical_formula_weight 905.66 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 11.0210(14) _cell_length_b 20.302(3) _cell_length_c 22.096(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.906(2) _cell_angle_gamma 90.00 _cell_volume 4799.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9837 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.53 _exptl_crystal_description block _exptl_crystal_colour reddish _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 1.840 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6770 _exptl_absorpt_correction_T_max 0.7330 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40943 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.54 _reflns_number_total 10962 _reflns_number_gt 8877 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Restraints have been applied to refine the tert-butyl group and THF molecule which are affected by disorder. DELU 0.01 C17 C14 C14' C15 C15' C16 C16' DELU 0.01 C2' C2 C1' C1 C3' C3 C4 DELU 0.01 O1 C43 C42 C41 C40 SIMU 0.01 C17 C14 C14' C15 C15' C16 C16' SIMU 0.01 C2' C2 C1' C1 C3' C3 C4 SIMU 0.01 O1 C43 C42 C41 C40 ; _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^)+(0.0575P)^2^+3.2793P] 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 10962 _refine_ls_number_parameters 555 _refine_ls_number_restraints 196 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.041 _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 C1 C 0.4110(11) 0.6575(8) 0.5750(4) 0.127(3) Uani 0.662(7) 1 d PDU A 1 H1A H 0.3551 0.6891 0.5860 0.191 Uiso 0.662(7) 1 calc PR A 1 H1B H 0.4946 0.6658 0.5989 0.191 Uiso 0.662(7) 1 calc PR A 1 H1C H 0.3861 0.6139 0.5837 0.191 Uiso 0.662(7) 1 calc PR A 1 C2 C 0.4953(9) 0.6128(6) 0.4869(6) 0.134(4) Uani 0.662(7) 1 d PDU A 1 H2A H 0.4463 0.5788 0.4623 0.200 Uiso 0.662(7) 1 calc PR A 1 H2B H 0.5498 0.5935 0.5231 0.200 Uiso 0.662(7) 1 calc PR A 1 H2C H 0.5443 0.6348 0.4626 0.200 Uiso 0.662(7) 1 calc PR A 1 C3 C 0.4551(7) 0.7302(4) 0.4968(5) 0.092(2) Uani 0.662(7) 1 d PDU A 1 H3A H 0.4025 0.7634 0.5080 0.138 Uiso 0.662(7) 1 calc PR A 1 H3B H 0.4550 0.7347 0.4536 0.138 Uiso 0.662(7) 1 calc PR A 1 H3C H 0.5388 0.7352 0.5218 0.138 Uiso 0.662(7) 1 calc PR A 1 C4 C 0.4068(4) 0.6634(3) 0.5078(2) 0.0701(11) Uani 1 1 d U . . C5 C 0.2729(4) 0.6500(2) 0.4722(2) 0.0604(9) Uani 1 1 d . A . C6 C 0.2169(5) 0.5892(2) 0.4617(3) 0.0873(15) Uani 1 1 d . . . H6 H 0.2555 0.5489 0.4736 0.105 Uiso 1 1 calc R A . C7 C 0.0928(5) 0.5981(2) 0.4303(3) 0.0843(14) Uani 1 1 d . A . H7 H 0.0329 0.5657 0.4167 0.101 Uiso 1 1 calc R . . C8 C 0.0771(4) 0.66582(19) 0.42342(19) 0.0579(9) Uani 1 1 d . . . C9 C -0.0384(4) 0.6996(2) 0.4029(2) 0.0616(10) Uani 1 1 d . A . H9 H -0.1099 0.6747 0.3873 0.074 Uiso 1 1 calc R . . C10 C -0.1811(4) 0.7898(2) 0.3869(2) 0.0662(11) Uani 1 1 d . A . C11 C -0.1722(5) 0.8603(3) 0.4092(3) 0.0838(14) Uani 1 1 d . . . H11A H -0.1476 0.8612 0.4540 0.126 Uiso 1 1 calc R . . H11B H -0.2521 0.8813 0.3952 0.126 Uiso 1 1 calc R . . H11C H -0.1112 0.8833 0.3927 0.126 Uiso 1 1 calc R . . C12 C -0.2304(4) 0.7864(3) 0.3165(2) 0.0839(14) Uani 1 1 d . . . H12A H -0.1745 0.8096 0.2967 0.126 Uiso 1 1 calc R . . H12B H -0.3117 0.8062 0.3050 0.126 Uiso 1 1 calc R . . H12C H -0.2359 0.7412 0.3034 0.126 Uiso 1 1 calc R . . C13 C -0.2684(5) 0.7509(3) 0.4187(3) 0.112(2) Uani 1 1 d . . . H13A H -0.2746 0.7062 0.4041 0.168 Uiso 1 1 calc R . . H13B H -0.3499 0.7707 0.4088 0.168 Uiso 1 1 calc R . . H13C H -0.2353 0.7514 0.4630 0.168 Uiso 1 1 calc R . . C14 C 0.1920(11) 0.7388(9) 0.2695(8) 0.089(4) Uani 0.512(19) 1 d PDU B 1 H14A H 0.1373 0.7633 0.2369 0.133 Uiso 0.512(19) 1 calc PR B 1 H14B H 0.1712 0.7479 0.3085 0.133 Uiso 0.512(19) 1 calc PR B 1 H14C H 0.1824 0.6926 0.2606 0.133 Uiso 0.512(19) 1 calc PR B 1 C15 C 0.4141(17) 0.7040(10) 0.3016(8) 0.096(4) Uani 0.512(19) 1 d PDU B 1 H15A H 0.4951 0.7143 0.2951 0.143 Uiso 0.512(19) 1 calc PR B 1 H15B H 0.3859 0.6628 0.2818 0.143 Uiso 0.512(19) 1 calc PR B 1 H15C H 0.4193 0.7007 0.3455 0.143 Uiso 0.512(19) 1 calc PR B 1 C16 C 0.3370(18) 0.7740(8) 0.2069(6) 0.096(4) Uani 0.512(19) 1 d PDU B 1 H16A H 0.4098 0.8009 0.2097 0.145 Uiso 0.512(19) 1 calc PR B 1 H16B H 0.2644 0.7971 0.1841 0.145 Uiso 0.512(19) 1 calc PR B 1 H16C H 0.3462 0.7336 0.1858 0.145 Uiso 0.512(19) 1 calc PR B 1 C17 C 0.3221(4) 0.7583(2) 0.27356(19) 0.0643(10) Uani 1 1 d U . . C18 C 0.3587(3) 0.81855(19) 0.31333(19) 0.0542(9) Uani 1 1 d . A . C19 C 0.4260(4) 0.8731(2) 0.3027(2) 0.0675(11) Uani 1 1 d . . . H19 H 0.4766 0.8755 0.2718 0.081 Uiso 1 1 calc R B . C20 C 0.4390(4) 0.9145(2) 0.3544(2) 0.0669(11) Uani 1 1 d . A . H20 H 0.5005 0.9500 0.3655 0.080 Uiso 1 1 calc R . . C21 C 0.3810(3) 0.88357(19) 0.39543(19) 0.0561(9) Uani 1 1 d . . . C22 C 0.3715(4) 0.9046(2) 0.4599(2) 0.0661(10) Uani 1 1 d . A . H22A H 0.4456 0.8902 0.4904 0.079 Uiso 1 1 calc R . . H22B H 0.3677 0.9523 0.4617 0.079 Uiso 1 1 calc R . . C23 C 0.2350(5) 0.9007(2) 0.5339(2) 0.0723(12) Uani 1 1 d . A . C24 C 0.1919(7) 0.9721(3) 0.5276(3) 0.118(2) Uani 1 1 d . . . H24A H 0.2583 0.9995 0.5207 0.177 Uiso 1 1 calc R . . H24B H 0.1697 0.9857 0.5652 0.177 Uiso 1 1 calc R . . H24C H 0.1205 0.9763 0.4930 0.177 Uiso 1 1 calc R . . C25 C 0.3496(5) 0.8949(4) 0.5893(2) 0.105(2) Uani 1 1 d . . . H25A H 0.3797 0.8504 0.5925 0.157 Uiso 1 1 calc R . . H25B H 0.3264 0.9069 0.6270 0.157 Uiso 1 1 calc R . . H25C H 0.4142 0.9240 0.5829 0.157 Uiso 1 1 calc R . . C26 C 0.1323(6) 0.8569(3) 0.5460(3) 0.1012(18) Uani 1 1 d . . . H26A H 0.0622 0.8578 0.5105 0.152 Uiso 1 1 calc R . . H26B H 0.1067 0.8726 0.5820 0.152 Uiso 1 1 calc R . . H26C H 0.1627 0.8126 0.5532 0.152 Uiso 1 1 calc R . . C27 C 0.1880(12) 1.0517(4) 0.3614(4) 0.192(5) Uani 1 1 d . . . H27A H 0.1081 1.0303 0.3504 0.287 Uiso 1 1 calc R . . H27B H 0.1940 1.0775 0.3984 0.287 Uiso 1 1 calc R . . H27C H 0.2530 1.0191 0.3690 0.287 Uiso 1 1 calc R . . C28 C 0.3095(7) 1.1442(4) 0.3322(5) 0.170(4) Uani 1 1 d . . . H28A H 0.3878 1.1226 0.3340 0.255 Uiso 1 1 calc R . . H28B H 0.3080 1.1601 0.3729 0.255 Uiso 1 1 calc R . . H28C H 0.3000 1.1805 0.3036 0.255 Uiso 1 1 calc R . . C29 C 0.0834(6) 1.1358(3) 0.2891(4) 0.118(2) Uani 1 1 d . . . H29A H 0.0927 1.1660 0.2571 0.177 Uiso 1 1 calc R . . H29B H 0.0688 1.1599 0.3240 0.177 Uiso 1 1 calc R . . H29C H 0.0139 1.1071 0.2731 0.177 Uiso 1 1 calc R . . C30 C 0.2020(5) 1.0951(2) 0.3098(3) 0.0950(17) Uani 1 1 d . B . C31 C 0.2209(4) 1.0567(2) 0.2542(3) 0.0766(13) Uani 1 1 d . . . C32 C 0.2977(5) 1.0722(3) 0.2144(4) 0.110(2) Uani 1 1 d . B . H32 H 0.3550 1.1066 0.2195 0.132 Uiso 1 1 calc R . . C33 C 0.2738(5) 1.0279(3) 0.1667(4) 0.110(2) Uani 1 1 d . . . H33 H 0.3110 1.0264 0.1331 0.132 Uiso 1 1 calc R B . C34 C 0.1824(4) 0.9850(2) 0.1781(2) 0.0688(11) Uani 1 1 d . A . C35 C 0.1123(4) 0.9370(2) 0.1368(2) 0.0699(11) Uani 1 1 d . . . H35 H 0.1386 0.9250 0.1013 0.084 Uiso 1 1 calc R B . C36 C -0.0607(5) 0.8630(2) 0.1015(2) 0.0767(12) Uani 1 1 d . . . C37 C -0.1346(6) 0.9021(3) 0.0462(3) 0.1000(18) Uani 1 1 d . B . H37A H -0.1836 0.9350 0.0605 0.150 Uiso 1 1 calc R . . H37B H -0.1890 0.8729 0.0178 0.150 Uiso 1 1 calc R . . H37C H -0.0781 0.9230 0.0252 0.150 Uiso 1 1 calc R . . C38 C -0.1487(7) 0.8285(3) 0.1346(3) 0.116(2) Uani 1 1 d . B . H38A H -0.1011 0.8020 0.1680 0.173 Uiso 1 1 calc R . . H38B H -0.2052 0.8009 0.1056 0.173 Uiso 1 1 calc R . . H38C H -0.1954 0.8608 0.1513 0.173 Uiso 1 1 calc R . . C39 C 0.0201(7) 0.8121(3) 0.0781(3) 0.119(3) Uani 1 1 d . B . H39A H 0.0757 0.8343 0.0574 0.178 Uiso 1 1 calc R . . H39B H -0.0327 0.7827 0.0493 0.178 Uiso 1 1 calc R . . H39C H 0.0680 0.7875 0.1128 0.178 Uiso 1 1 calc R . . C40 C -0.2542(8) 1.0191(5) 0.1775(4) 0.146(2) Uani 1 1 d U B . H40A H -0.2463 0.9981 0.1392 0.175 Uiso 1 1 calc R . . H40B H -0.2354 1.0656 0.1752 0.175 Uiso 1 1 calc R . . C41 C -0.3778(8) 1.0108(6) 0.1855(5) 0.175(3) Uani 1 1 d U . . H41A H -0.4258 1.0510 0.1752 0.210 Uiso 1 1 calc R . . H41B H -0.4206 0.9754 0.1593 0.210 Uiso 1 1 calc R . . C42 C -0.3615(8) 0.9954(6) 0.2479(5) 0.181(3) Uani 1 1 d U . . H42A H -0.3991 0.9531 0.2525 0.218 Uiso 1 1 calc R . . H42B H -0.4002 1.0287 0.2686 0.218 Uiso 1 1 calc R . . C43 C -0.2312(8) 0.9933(5) 0.2739(4) 0.165(3) Uani 1 1 d U B . H43A H -0.2050 1.0322 0.2992 0.198 Uiso 1 1 calc R . . H43B H -0.2102 0.9548 0.3003 0.198 Uiso 1 1 calc R . . C1' C 0.4535(18) 0.6078(10) 0.5536(10) 0.111(5) Uani 0.338(7) 1 d PDU A 2 H1'A H 0.4193 0.6129 0.5895 0.166 Uiso 0.338(7) 1 calc PR A 2 H1'B H 0.5431 0.6093 0.5664 0.166 Uiso 0.338(7) 1 calc PR A 2 H1'C H 0.4275 0.5663 0.5340 0.166 Uiso 0.338(7) 1 calc PR A 2 C2' C 0.4827(16) 0.6717(12) 0.4625(9) 0.109(4) Uani 0.338(7) 1 d PDU A 2 H2'A H 0.4690 0.7149 0.4443 0.163 Uiso 0.338(7) 1 calc PR A 2 H2'B H 0.4596 0.6391 0.4303 0.163 Uiso 0.338(7) 1 calc PR A 2 H2'C H 0.5695 0.6667 0.4830 0.163 Uiso 0.338(7) 1 calc PR A 2 C3' C 0.4136(17) 0.7263(10) 0.5484(10) 0.111(5) Uani 0.338(7) 1 d PDU A 2 H3'A H 0.3305 0.7410 0.5478 0.166 Uiso 0.338(7) 1 calc PR A 2 H3'B H 0.4572 0.7604 0.5321 0.166 Uiso 0.338(7) 1 calc PR A 2 H3'C H 0.4573 0.7165 0.5905 0.166 Uiso 0.338(7) 1 calc PR A 2 C14' C 0.2225(13) 0.7159(8) 0.2976(7) 0.075(3) Uani 0.488(19) 1 d PDU B 2 H14D H 0.2433 0.7159 0.3424 0.112 Uiso 0.488(19) 1 calc PR B 2 H14E H 0.2230 0.6715 0.2827 0.112 Uiso 0.488(19) 1 calc PR B 2 H14F H 0.1409 0.7347 0.2824 0.112 Uiso 0.488(19) 1 calc PR B 2 C15' C 0.4344(14) 0.7123(11) 0.2766(10) 0.094(4) Uani 0.488(19) 1 d PDU B 2 H15D H 0.4985 0.7356 0.2627 0.141 Uiso 0.488(19) 1 calc PR B 2 H15E H 0.4082 0.6749 0.2502 0.141 Uiso 0.488(19) 1 calc PR B 2 H15F H 0.4665 0.6978 0.3187 0.141 Uiso 0.488(19) 1 calc PR B 2 C16' C 0.2583(19) 0.7751(8) 0.2071(6) 0.099(4) Uani 0.488(19) 1 d PDU B 2 H16D H 0.3137 0.8009 0.1891 0.148 Uiso 0.488(19) 1 calc PR B 2 H16E H 0.1837 0.7998 0.2063 0.148 Uiso 0.488(19) 1 calc PR B 2 H16F H 0.2370 0.7352 0.1836 0.148 Uiso 0.488(19) 1 calc PR B 2 Cl1 Cl 0.04922(10) 0.88004(7) 0.31382(6) 0.0843(4) Uani 1 1 d . . . Er1 Er 0.160484(14) 0.806053(7) 0.411572(7) 0.04644(7) Uani 1 1 d . A . Li1 Li -0.0147(7) 0.9549(4) 0.2254(4) 0.0686(18) Uani 1 1 d . A . Li2 Li 0.2354(7) 0.9271(4) 0.2948(4) 0.0736(19) Uani 1 1 d . A . N1 N 0.1889(3) 0.69770(14) 0.44924(16) 0.0532(7) Uani 1 1 d . A . N2 N -0.0503(3) 0.76219(16) 0.40460(15) 0.0558(7) Uani 1 1 d . . . N3 N 0.3304(3) 0.82514(15) 0.37058(14) 0.0517(7) Uani 1 1 d . A . N4 N 0.2609(3) 0.87669(16) 0.47542(14) 0.0558(7) Uani 1 1 d . . . N5 N 0.1502(3) 1.00322(17) 0.23191(18) 0.0676(9) Uani 1 1 d . A . N6 N 0.0141(3) 0.90989(17) 0.14730(16) 0.0647(8) Uani 1 1 d . A . O1 O -0.1731(3) 0.9908(2) 0.22771(17) 0.1004(12) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.101(7) 0.188(9) 0.080(5) 0.028(6) -0.003(4) -0.028(7) C2 0.069(5) 0.132(7) 0.186(8) -0.032(7) 0.005(6) 0.034(5) C3 0.061(4) 0.102(5) 0.100(6) 0.011(4) -0.006(4) -0.012(4) C4 0.049(2) 0.085(3) 0.073(3) 0.012(2) 0.0081(19) 0.007(2) C5 0.054(2) 0.056(2) 0.070(2) 0.0024(18) 0.0148(19) 0.0052(18) C6 0.073(3) 0.058(3) 0.123(4) -0.002(3) 0.008(3) 0.009(2) C7 0.071(3) 0.056(3) 0.118(4) -0.012(3) 0.007(3) -0.010(2) C8 0.050(2) 0.051(2) 0.071(2) -0.0057(18) 0.0099(18) -0.0092(17) C9 0.045(2) 0.064(3) 0.073(3) -0.0017(19) 0.0091(18) -0.0092(17) C10 0.039(2) 0.079(3) 0.081(3) 0.010(2) 0.0134(19) 0.0019(18) C11 0.065(3) 0.092(4) 0.095(4) -0.004(3) 0.021(3) 0.019(3) C12 0.052(3) 0.095(3) 0.091(4) 0.000(3) -0.009(2) 0.002(2) C13 0.048(3) 0.147(6) 0.146(5) 0.055(4) 0.035(3) 0.005(3) C14 0.063(5) 0.109(9) 0.093(9) -0.028(7) 0.014(5) -0.025(5) C15 0.095(8) 0.086(7) 0.098(9) -0.017(7) 0.010(7) 0.016(6) C16 0.098(9) 0.122(8) 0.073(5) -0.010(5) 0.027(6) -0.001(8) C17 0.053(2) 0.079(3) 0.060(2) -0.0090(19) 0.0103(17) 0.0055(18) C18 0.0355(17) 0.065(2) 0.062(2) 0.0058(17) 0.0115(16) 0.0020(15) C19 0.048(2) 0.079(3) 0.082(3) 0.014(2) 0.028(2) -0.003(2) C20 0.048(2) 0.064(2) 0.090(3) 0.007(2) 0.020(2) -0.0122(19) C21 0.0421(19) 0.055(2) 0.068(2) -0.0012(17) 0.0080(17) -0.0067(16) C22 0.057(2) 0.059(2) 0.079(3) -0.009(2) 0.008(2) -0.0126(18) C23 0.081(3) 0.070(3) 0.061(2) -0.015(2) 0.008(2) -0.003(2) C24 0.153(6) 0.091(4) 0.118(5) -0.022(4) 0.049(5) 0.028(4) C25 0.101(5) 0.129(5) 0.071(3) -0.026(3) -0.005(3) -0.007(3) C26 0.103(4) 0.134(5) 0.076(3) -0.023(3) 0.039(3) -0.028(4) C27 0.368(16) 0.101(5) 0.105(5) 0.011(4) 0.054(8) 0.073(8) C28 0.110(6) 0.150(7) 0.214(9) -0.049(7) -0.033(6) -0.022(5) C29 0.096(4) 0.100(4) 0.149(6) -0.019(4) 0.009(4) 0.028(4) C30 0.084(4) 0.061(3) 0.120(4) -0.007(3) -0.015(3) 0.008(2) C31 0.055(3) 0.057(2) 0.105(4) 0.006(2) -0.005(2) 0.0063(19) C32 0.063(3) 0.088(4) 0.179(7) 0.001(4) 0.030(4) -0.020(3) C33 0.068(3) 0.111(5) 0.166(6) 0.005(5) 0.056(4) -0.007(3) C34 0.050(2) 0.072(3) 0.085(3) 0.013(2) 0.017(2) 0.0068(19) C35 0.064(3) 0.076(3) 0.073(3) 0.009(2) 0.023(2) 0.016(2) C36 0.074(3) 0.069(3) 0.081(3) -0.013(2) 0.007(2) 0.008(2) C37 0.091(4) 0.096(4) 0.096(4) -0.006(3) -0.009(3) 0.019(3) C38 0.122(6) 0.098(4) 0.127(5) -0.014(4) 0.029(4) -0.032(4) C39 0.113(5) 0.110(5) 0.118(5) -0.046(4) -0.005(4) 0.046(4) C40 0.128(5) 0.200(6) 0.115(4) 0.039(4) 0.041(4) 0.066(5) C41 0.102(4) 0.254(7) 0.154(5) -0.023(6) 0.004(4) 0.044(5) C42 0.111(4) 0.258(7) 0.195(6) 0.054(6) 0.076(5) 0.014(5) C43 0.134(5) 0.249(6) 0.123(4) 0.050(5) 0.055(4) 0.087(5) C1' 0.074(8) 0.123(8) 0.115(9) 0.044(7) -0.019(7) 0.007(8) C2' 0.057(7) 0.154(10) 0.113(8) 0.020(8) 0.018(6) -0.007(8) C3' 0.083(8) 0.118(8) 0.107(9) -0.012(7) -0.023(7) -0.004(8) C14' 0.067(6) 0.080(7) 0.074(7) -0.024(5) 0.009(5) -0.015(5) C15' 0.071(6) 0.100(8) 0.103(11) -0.023(8) 0.006(6) 0.017(6) C16' 0.108(10) 0.120(8) 0.062(5) 0.001(5) 0.007(6) 0.020(8) Cl1 0.0532(6) 0.1039(9) 0.0931(8) 0.0463(7) 0.0125(5) 0.0059(6) Er1 0.04179(10) 0.04619(10) 0.04976(10) -0.00041(6) 0.00793(7) -0.00754(6) Li1 0.056(4) 0.081(5) 0.071(4) 0.001(4) 0.018(3) 0.006(3) Li2 0.054(4) 0.078(5) 0.085(5) 0.011(4) 0.008(4) 0.003(3) N1 0.0423(16) 0.0542(18) 0.0611(19) -0.0003(13) 0.0085(14) -0.0029(13) N2 0.0379(15) 0.0603(19) 0.0666(19) 0.0042(15) 0.0073(13) -0.0043(13) N3 0.0435(16) 0.0551(16) 0.0542(17) -0.0019(13) 0.0074(13) -0.0086(13) N4 0.0509(18) 0.0578(18) 0.0557(18) -0.0060(14) 0.0068(14) -0.0069(14) N5 0.063(2) 0.059(2) 0.077(2) 0.0104(17) 0.0094(18) -0.0031(16) N6 0.056(2) 0.069(2) 0.068(2) -0.0032(16) 0.0126(16) 0.0052(16) O1 0.080(2) 0.146(3) 0.082(2) 0.026(2) 0.0327(18) 0.048(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C4 1.480(10) . ? C2 C4 1.562(10) . ? C3 C4 1.497(10) . ? C4 C2' 1.461(17) . ? C4 C1' 1.522(16) . ? C4 C5 1.520(6) . ? C4 C3' 1.553(18) . ? C5 N1 1.352(5) . ? C5 C6 1.375(6) . ? C6 C7 1.389(7) . ? C7 C8 1.389(6) . ? C8 N1 1.387(5) . ? C8 C9 1.421(6) . ? C9 N2 1.278(5) . ? C10 N2 1.508(5) . ? C10 C11 1.510(7) . ? C10 C12 1.521(7) . ? C10 C13 1.539(6) . ? C14 C17 1.469(12) . ? C15 C17 1.525(16) . ? C16 C17 1.553(12) . ? C17 C16' 1.506(12) . ? C17 C18 1.504(6) . ? C17 C15' 1.538(16) . ? C17 C14' 1.583(13) . ? C18 N3 1.380(5) . ? C18 C19 1.385(5) . ? C18 Li2 2.570(9) . ? C19 C20 1.398(6) . ? C19 Li2 2.339(9) . ? C20 C21 1.379(5) . ? C20 Li2 2.328(9) . ? C21 N3 1.368(5) . ? C21 C22 1.515(6) . ? C21 Li2 2.566(9) . ? C22 N4 1.458(5) . ? C23 N4 1.472(5) . ? C23 C26 1.512(7) . ? C23 C24 1.523(7) . ? C23 C25 1.537(6) . ? C27 C30 1.477(10) . ? C28 C30 1.537(9) . ? C29 C30 1.520(8) . ? C30 C31 1.512(8) . ? C31 N5 1.358(6) . ? C31 C32 1.396(8) . ? C31 Li2 2.771(9) . ? C32 C33 1.363(9) . ? C33 C34 1.400(7) . ? C34 N5 1.370(6) . ? C34 C35 1.429(7) . ? C34 Li2 2.765(9) . ? C35 N6 1.285(6) . ? C36 N6 1.486(6) . ? C36 C38 1.520(8) . ? C36 C37 1.520(7) . ? C36 C39 1.533(7) . ? C40 O1 1.371(8) . ? C40 C41 1.425(11) . ? C41 C42 1.383(11) . ? C42 C43 1.414(11) . ? C43 O1 1.330(8) . ? Cl1 Li2 2.390(8) . ? Cl1 Li1 2.442(8) . ? Cl1 Er1 2.6743(11) . ? Er1 N4 2.126(3) . ? Er1 N3 2.300(3) . ? Er1 N1 2.346(3) . ? Er1 N2 2.458(3) . ? Li1 O1 1.904(8) . ? Li1 N6 2.044(8) . ? Li1 N5 2.040(8) . ? Li1 Li2 2.869(11) . ? Li2 N5 2.138(8) . ? Li2 N3 2.710(8) . ? 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 C2' C4 C1 144.3(9) . . ? C2' C4 C3 60.0(10) . . ? C1 C4 C3 108.0(7) . . ? C2' C4 C1' 112.6(12) . . ? C1 C4 C1' 49.2(9) . . ? C3 C4 C1' 134.6(9) . . ? C2' C4 C5 108.2(8) . . ? C1 C4 C5 107.3(5) . . ? C3 C4 C5 114.7(4) . . ? C1' C4 C5 110.0(8) . . ? C2' C4 C2 51.1(9) . . ? C1 C4 C2 111.8(8) . . ? C3 C4 C2 106.0(7) . . ? C1' C4 C2 64.7(10) . . ? C5 C4 C2 109.1(5) . . ? C2' C4 C3' 110.2(13) . . ? C1 C4 C3' 60.0(10) . . ? C3 C4 C3' 51.7(9) . . ? C1' C4 C3' 105.2(12) . . ? C5 C4 C3' 110.6(7) . . ? C2 C4 C3' 140.0(9) . . ? N1 C5 C6 109.9(4) . . ? N1 C5 C4 123.9(4) . . ? C6 C5 C4 126.1(4) . . ? C5 C6 C7 108.4(4) . . ? C6 C7 C8 105.4(4) . . ? N1 C8 C7 110.0(4) . . ? N1 C8 C9 123.0(3) . . ? C7 C8 C9 126.2(4) . . ? N2 C9 C8 124.1(4) . . ? N2 C10 C11 106.6(3) . . ? N2 C10 C12 109.4(4) . . ? C11 C10 C12 110.9(4) . . ? N2 C10 C13 110.8(4) . . ? C11 C10 C13 109.7(4) . . ? C12 C10 C13 109.5(4) . . ? C14 C17 C16' 77.4(8) . . ? C14 C17 C18 112.0(6) . . ? C16' C17 C18 112.5(7) . . ? C14 C17 C15 112.0(10) . . ? C16' C17 C15 131.9(9) . . ? C18 C17 C15 107.0(8) . . ? C14 C17 C15' 127.1(11) . . ? C16' C17 C15' 111.2(9) . . ? C18 C17 C15' 111.6(9) . . ? C15 C17 C15' 25.1(8) . . ? C14 C17 C16 108.8(8) . . ? C16' C17 C16 32.9(6) . . ? C18 C17 C16 108.2(6) . . ? C15 C17 C16 108.7(8) . . ? C15' C17 C16 84.1(8) . . ? C14 C17 C14' 29.5(6) . . ? C16' C17 C14' 104.6(8) . . ? C18 C17 C14' 110.8(5) . . ? C15 C17 C14' 85.3(9) . . ? C15' C17 C14' 105.8(9) . . ? C16 C17 C14' 132.1(7) . . ? N3 C18 C19 109.1(4) . . ? N3 C18 C17 121.8(3) . . ? C19 C18 C17 129.1(4) . . ? N3 C18 Li2 80.5(3) . . ? C19 C18 Li2 64.6(3) . . ? C17 C18 Li2 123.2(3) . . ? C18 C19 C20 107.1(4) . . ? C18 C19 Li2 83.0(3) . . ? C20 C19 Li2 72.1(3) . . ? C21 C20 C19 107.0(4) . . ? C21 C20 Li2 83.4(3) . . ? C19 C20 Li2 73.0(3) . . ? N3 C21 C20 109.8(4) . . ? N3 C21 C22 120.5(3) . . ? C20 C21 C22 129.6(4) . . ? N3 C21 Li2 80.9(3) . . ? C20 C21 Li2 64.3(3) . . ? C22 C21 Li2 123.2(3) . . ? N4 C22 C21 111.2(3) . . ? N4 C23 C26 105.8(4) . . ? N4 C23 C24 110.9(4) . . ? C26 C23 C24 110.2(5) . . ? N4 C23 C25 112.2(4) . . ? C26 C23 C25 108.7(5) . . ? C24 C23 C25 108.8(5) . . ? C27 C30 C31 112.4(5) . . ? C27 C30 C28 110.7(7) . . ? C31 C30 C28 110.4(6) . . ? C27 C30 C29 108.4(7) . . ? C31 C30 C29 108.2(5) . . ? C28 C30 C29 106.6(5) . . ? N5 C31 C32 109.5(5) . . ? N5 C31 C30 121.9(5) . . ? C32 C31 C30 128.3(5) . . ? N5 C31 Li2 48.9(3) . . ? C32 C31 Li2 115.0(4) . . ? C30 C31 Li2 103.6(4) . . ? C33 C32 C31 107.7(5) . . ? C32 C33 C34 106.5(6) . . ? N5 C34 C33 109.7(5) . . ? N5 C34 C35 121.8(4) . . ? C33 C34 C35 127.6(5) . . ? N5 C34 Li2 49.2(3) . . ? C33 C34 Li2 115.6(4) . . ? C35 C34 Li2 105.5(3) . . ? N6 C35 C34 121.7(4) . . ? N6 C36 C38 106.3(4) . . ? N6 C36 C37 108.4(4) . . ? C38 C36 C37 110.3(5) . . ? N6 C36 C39 112.9(4) . . ? C38 C36 C39 110.0(5) . . ? C37 C36 C39 108.8(5) . . ? O1 C40 C41 107.9(7) . . ? C42 C41 C40 104.5(7) . . ? C41 C42 C43 106.7(7) . . ? O1 C43 C42 108.6(7) . . ? Li2 Cl1 Li1 72.9(3) . . ? Li2 Cl1 Er1 96.91(19) . . ? Li1 Cl1 Er1 169.73(18) . . ? N4 Er1 N3 78.74(12) . . ? N4 Er1 N1 113.15(12) . . ? N3 Er1 N1 104.23(11) . . ? N4 Er1 N2 128.26(12) . . ? N3 Er1 N2 151.98(11) . . ? N1 Er1 N2 74.10(11) . . ? N4 Er1 Cl1 102.81(10) . . ? N3 Er1 Cl1 81.14(8) . . ? N1 Er1 Cl1 144.03(9) . . ? N2 Er1 Cl1 84.83(8) . . ? O1 Li1 N6 121.5(4) . . ? O1 Li1 N5 128.4(5) . . ? N6 Li1 N5 87.6(3) . . ? O1 Li1 Cl1 107.9(3) . . ? N6 Li1 Cl1 108.9(3) . . ? N5 Li1 Cl1 99.3(3) . . ? O1 Li1 Li2 146.1(4) . . ? N6 Li1 Li2 92.3(3) . . ? N5 Li1 Li2 48.1(2) . . ? Cl1 Li1 Li2 52.8(2) . . ? N5 Li2 C20 131.3(4) . . ? N5 Li2 C19 129.3(4) . . ? C20 Li2 C19 34.87(19) . . ? N5 Li2 Cl1 98.2(3) . . ? C20 Li2 Cl1 127.4(4) . . ? C19 Li2 Cl1 126.4(4) . . ? N5 Li2 C21 153.8(4) . . ? C20 Li2 C21 32.26(16) . . ? C19 Li2 C21 53.9(2) . . ? Cl1 Li2 C21 95.4(3) . . ? N5 Li2 C18 148.9(4) . . ? C20 Li2 C18 54.1(2) . . ? C19 Li2 C18 32.34(17) . . ? Cl1 Li2 C18 94.1(3) . . ? C21 Li2 C18 50.94(19) . . ? N5 Li2 N3 176.1(4) . . ? C20 Li2 N3 52.34(19) . . ? C19 Li2 N3 52.4(2) . . ? Cl1 Li2 N3 78.8(2) . . ? C21 Li2 N3 29.90(13) . . ? C18 Li2 N3 30.15(14) . . ? N5 Li2 C34 29.02(17) . . ? C20 Li2 C34 122.3(3) . . ? C19 Li2 C34 104.7(3) . . ? Cl1 Li2 C34 109.6(3) . . ? C21 Li2 C34 154.5(3) . . ? C18 Li2 C34 119.9(3) . . ? N3 Li2 C34 149.8(4) . . ? N5 Li2 C31 28.57(17) . . ? C20 Li2 C31 105.1(3) . . ? C19 Li2 C31 116.7(3) . . ? Cl1 Li2 C31 116.8(3) . . ? C21 Li2 C31 125.6(3) . . ? C18 Li2 C31 148.5(4) . . ? N3 Li2 C31 155.3(3) . . ? C34 Li2 C31 46.5(2) . . ? N5 Li2 Li1 45.2(2) . . ? C20 Li2 Li1 174.7(4) . . ? C19 Li2 Li1 149.6(4) . . ? Cl1 Li2 Li1 54.4(2) . . ? C21 Li2 Li1 148.3(4) . . ? C18 Li2 Li1 131.1(4) . . ? N3 Li2 Li1 131.2(3) . . ? C34 Li2 Li1 57.2(2) . . ? C31 Li2 Li1 70.6(3) . . ? C5 N1 C8 106.3(3) . . ? C5 N1 Er1 145.7(3) . . ? C8 N1 Er1 105.2(2) . . ? C9 N2 C10 117.4(3) . . ? C9 N2 Er1 105.1(3) . . ? C10 N2 Er1 135.4(3) . . ? C21 N3 C18 107.0(3) . . ? C21 N3 Er1 106.2(2) . . ? C18 N3 Er1 136.8(2) . . ? C21 N3 Li2 69.2(3) . . ? C18 N3 Li2 69.3(3) . . ? Er1 N3 Li2 98.2(2) . . ? C22 N4 C23 115.3(3) . . ? C22 N4 Er1 115.9(2) . . ? C23 N4 Er1 128.8(3) . . ? C31 N5 C34 106.6(4) . . ? C31 N5 Li1 146.5(4) . . ? C34 N5 Li1 102.8(4) . . ? C31 N5 Li2 102.6(4) . . ? C34 N5 Li2 101.8(4) . . ? Li1 N5 Li2 86.7(3) . . ? C35 N6 C36 120.3(4) . . ? C35 N6 Li1 105.7(4) . . ? C36 N6 Li1 133.5(4) . . ? C43 O1 C40 105.3(5) . . ? C43 O1 Li1 130.5(5) . . ? C40 O1 Li1 124.2(5) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.465 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.071 data_3a _database_code_depnum_ccdc_archive 'CCDC 896986' #TrackingRef 'CCDC 896986.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H44 N5 Si2 Y' _chemical_formula_weight 547.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2007(12) _cell_length_b 9.3829(12) _cell_length_c 19.864(3) _cell_angle_alpha 88.008(2) _cell_angle_beta 84.805(2) _cell_angle_gamma 85.998(2) _cell_volume 1702.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3230 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 20.70 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 1.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5557 _exptl_absorpt_correction_T_max 0.7037 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13222 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0916 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6612 _reflns_number_gt 3626 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Some highly disordered solvent peaks of solvent molecule were observed but could not be modelled satisfactorily. The SQUEEZE routine in PLATON was used to modify the HKL file. Restraints have been applied to refine the ligand which is affected by disorder. sadi 0.01 c15A c16a c15B c16b c15A c17a c15B c17b c15A c18a c15B c18b sadi 0.01 c6A c7a c6A c8a c6A c9a c6B c7b c6B c8b c6B c9b sadi 0.01 C13B C14B C13A C14A C4A C5A C4B C5B sadi 0.01 c10a c11a c10b c11b c11a c12a c11b c12b c12a c13a c12b c13b sadi 0.01 c1a c2a c2a c3a c3a c4a c1b c2b c2b c3b c3b c4b sadi 0.01 n1a c4a n1a c1a n1b c4b n1b c1b n3a c13a n3a c10a n3b c13b n3b c10b sadi 0.01 n3a c14a n3b c14b sadi 0.01 c10a c12a c10b c12b c10a c13a c10b c13b sadi 0.01 c5a n2a c5b n2B c14a n4a c14b n4b sadi 0.01 Y1 N1A Y1 N1b Y1 N3A Y1 N3b DELU 0.01 $C DELU 0.01 $N SIMU 0.01 $C SIMU 0.01 $N ; _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^)+(0.0723P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6612 _refine_ls_number_parameters 485 _refine_ls_number_restraints 579 _refine_ls_R_factor_all 0.1099 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1429 _refine_ls_wR_factor_gt 0.1280 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.002 0.500 278 48 ' ' 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 C19 C 0.3149(8) 0.4347(7) 0.2835(3) 0.135(3) Uani 1 1 d . . . H19A H 0.2502 0.3675 0.3050 0.203 Uiso 1 1 calc R . . H19B H 0.3884 0.3852 0.2539 0.203 Uiso 1 1 calc R . . H19C H 0.2602 0.5046 0.2578 0.203 Uiso 1 1 calc R . . C20 C 0.5014(8) 0.3793(7) 0.3978(3) 0.145(3) Uani 1 1 d . . . H20A H 0.4437 0.3588 0.4393 0.217 Uiso 1 1 calc R . . H20B H 0.5945 0.4094 0.4077 0.217 Uiso 1 1 calc R . . H20C H 0.5158 0.2950 0.3713 0.217 Uiso 1 1 calc R . . C21 C 0.2542(7) 0.6034(8) 0.4086(3) 0.142(3) Uani 1 1 d . . . H21A H 0.2420 0.5418 0.4481 0.213 Uiso 1 1 calc R . . H21B H 0.1649 0.6128 0.3869 0.213 Uiso 1 1 calc R . . H21C H 0.2785 0.6958 0.4217 0.213 Uiso 1 1 calc R . . C22 C 0.7164(8) 0.8699(8) 0.2875(3) 0.140(3) Uani 1 1 d . . . H22A H 0.7730 0.9324 0.3101 0.210 Uiso 1 1 calc R . . H22B H 0.6483 0.9259 0.2618 0.210 Uiso 1 1 calc R . . H22C H 0.7804 0.8106 0.2576 0.210 Uiso 1 1 calc R . . C23 C 0.7568(9) 0.6583(9) 0.4003(4) 0.172(3) Uani 1 1 d . . . H23A H 0.7618 0.7055 0.4421 0.258 Uiso 1 1 calc R . . H23B H 0.8504 0.6575 0.3746 0.258 Uiso 1 1 calc R . . H23C H 0.7307 0.5619 0.4097 0.258 Uiso 1 1 calc R . . C24 C 0.5036(9) 0.8793(8) 0.4109(4) 0.161(3) Uani 1 1 d . . . H24A H 0.5539 0.8871 0.4508 0.241 Uiso 1 1 calc R . . H24B H 0.4102 0.8416 0.4231 0.241 Uiso 1 1 calc R . . H24C H 0.4897 0.9721 0.3896 0.241 Uiso 1 1 calc R . . C1A C 0.2682(7) 0.5826(8) 0.0910(4) 0.0777(19) Uani 0.785(3) 1 d PDU A 1 H1AA H 0.1998 0.6587 0.1004 0.093 Uiso 0.785(3) 1 calc PR A 1 C2A C 0.2527(8) 0.4757(8) 0.0453(4) 0.0770(17) Uani 0.785(3) 1 d PDU A 1 H2AA H 0.1758 0.4701 0.0183 0.092 Uiso 0.785(3) 1 calc PR A 1 C3A C 0.3744(7) 0.3792(8) 0.0479(4) 0.0743(18) Uani 0.785(3) 1 d PDU A 1 H3AA H 0.3962 0.2972 0.0229 0.089 Uiso 0.785(3) 1 calc PR A 1 C4A C 0.4570(9) 0.4328(8) 0.0963(5) 0.0634(17) Uani 0.785(3) 1 d PDU A 1 C5A C 0.5879(6) 0.3770(6) 0.1180(3) 0.0700(15) Uani 0.785(3) 1 d PDU A 1 H5AA H 0.6275 0.2902 0.1010 0.084 Uiso 0.785(3) 1 calc PR A 1 C6A C 0.7989(10) 0.3704(9) 0.1809(4) 0.085(2) Uani 0.785(3) 1 d PDU A 1 C7A C 0.9079(18) 0.333(2) 0.1202(5) 0.109(4) Uani 0.785(3) 1 d PDU A 1 H7AA H 0.9293 0.4180 0.0942 0.164 Uiso 0.785(3) 1 calc PR A 1 H7AB H 0.8663 0.2674 0.0923 0.164 Uiso 0.785(3) 1 calc PR A 1 H7AC H 0.9966 0.2888 0.1359 0.164 Uiso 0.785(3) 1 calc PR A 1 C8A C 0.7697(9) 0.2309(8) 0.2204(4) 0.110(2) Uani 0.785(3) 1 d PDU A 1 H8AA H 0.7013 0.2505 0.2589 0.166 Uiso 0.785(3) 1 calc PR A 1 H8AB H 0.8596 0.1885 0.2353 0.166 Uiso 0.785(3) 1 calc PR A 1 H8AC H 0.7297 0.1662 0.1917 0.166 Uiso 0.785(3) 1 calc PR A 1 C9A C 0.8548(8) 0.4731(8) 0.2290(4) 0.107(2) Uani 0.785(3) 1 d PDU A 1 H9AA H 0.8747 0.5614 0.2052 0.161 Uiso 0.785(3) 1 calc PR A 1 H9AB H 0.9429 0.4314 0.2461 0.161 Uiso 0.785(3) 1 calc PR A 1 H9AC H 0.7820 0.4911 0.2660 0.161 Uiso 0.785(3) 1 calc PR A 1 C10A C 0.8174(7) 0.7796(8) 0.0873(4) 0.0662(19) Uani 0.785(3) 1 d PDU A 1 H10B H 0.8878 0.7058 0.0942 0.079 Uiso 0.785(3) 1 calc PR A 1 C11A C 0.8371(8) 0.8904(8) 0.0402(4) 0.0736(19) Uani 0.785(3) 1 d PDU A 1 H11B H 0.9195 0.9053 0.0108 0.088 Uiso 0.785(3) 1 calc PR A 1 C12A C 0.7064(7) 0.9742(8) 0.0465(4) 0.0799(19) Uani 0.785(3) 1 d PDU A 1 H12B H 0.6843 1.0569 0.0212 0.096 Uiso 0.785(3) 1 calc PR A 1 C13A C 0.6144(7) 0.9129(7) 0.0972(4) 0.0667(16) Uani 0.785(3) 1 d PDU A 1 C14A C 0.4738(7) 0.9586(6) 0.1228(3) 0.0684(15) Uani 0.785(3) 1 d PDU A 1 H14A H 0.4311 1.0433 0.1056 0.082 Uiso 0.785(3) 1 calc PR A 1 C15A C 0.2532(10) 0.9479(9) 0.1973(4) 0.0876(19) Uani 0.785(3) 1 d PDU A 1 C16A C 0.1827(8) 0.8352(8) 0.2439(4) 0.106(2) Uani 0.785(3) 1 d PDU A 1 H16A H 0.2437 0.8102 0.2798 0.160 Uiso 0.785(3) 1 calc PR A 1 H16B H 0.1716 0.7518 0.2187 0.160 Uiso 0.785(3) 1 calc PR A 1 H16C H 0.0885 0.8726 0.2626 0.160 Uiso 0.785(3) 1 calc PR A 1 C17A C 0.1570(10) 0.9891(10) 0.1396(5) 0.117(3) Uani 0.785(3) 1 d PDU A 1 H17A H 0.2022 1.0604 0.1105 0.175 Uiso 0.785(3) 1 calc PR A 1 H17B H 0.0626 1.0266 0.1580 0.175 Uiso 0.785(3) 1 calc PR A 1 H17C H 0.1460 0.9061 0.1140 0.175 Uiso 0.785(3) 1 calc PR A 1 C18A C 0.2753(10) 1.0809(9) 0.2363(5) 0.133(3) Uani 0.785(3) 1 d PDU A 1 H18A H 0.3204 1.1504 0.2062 0.200 Uiso 0.785(3) 1 calc PR A 1 H18B H 0.3370 1.0555 0.2719 0.200 Uiso 0.785(3) 1 calc PR A 1 H18C H 0.1823 1.1206 0.2554 0.200 Uiso 0.785(3) 1 calc PR A 1 C1B C 0.623(2) 0.956(2) 0.0896(17) 0.070(3) Uani 0.215(3) 1 d PGDU A 2 H1BA H 0.5402 1.0185 0.0944 0.084 Uiso 0.215(3) 1 calc PR A 2 C2B C 0.752(3) 0.973(3) 0.0463(14) 0.072(3) Uani 0.215(3) 1 d PGDU A 2 H2BA H 0.7701 1.0511 0.0171 0.086 Uiso 0.215(3) 1 calc PR A 2 C3B C 0.850(2) 0.852(3) 0.0554(15) 0.067(3) Uani 0.215(3) 1 d PGDU A 2 H3BA H 0.9428 0.8356 0.0333 0.081 Uiso 0.215(3) 1 calc PR A 2 C4B C 0.781(4) 0.759(2) 0.1044(18) 0.064(3) Uani 0.215(3) 1 d PGDU A 2 C5B C 0.8447(19) 0.6269(15) 0.1194(9) 0.062(3) Uani 0.215(3) 1 d PDU A 2 H5BA H 0.9365 0.5941 0.1003 0.074 Uiso 0.215(3) 1 calc PR A 2 C6B C 0.829(3) 0.398(5) 0.1805(14) 0.090(4) Uani 0.215(3) 1 d PDU A 2 C7B C 0.883(7) 0.353(8) 0.1088(19) 0.093(6) Uani 0.215(3) 1 d PDU A 2 H7BA H 0.9514 0.4185 0.0889 0.140 Uiso 0.215(3) 1 calc PR A 2 H7BB H 0.8020 0.3521 0.0818 0.140 Uiso 0.215(3) 1 calc PR A 2 H7BC H 0.9312 0.2584 0.1107 0.140 Uiso 0.215(3) 1 calc PR A 2 C8B C 0.960(3) 0.426(3) 0.2190(15) 0.105(6) Uani 0.215(3) 1 d PDU A 2 H8BA H 1.0289 0.4776 0.1901 0.158 Uiso 0.215(3) 1 calc PR A 2 H8BB H 1.0069 0.3360 0.2329 0.158 Uiso 0.215(3) 1 calc PR A 2 H8BC H 0.9281 0.4804 0.2581 0.158 Uiso 0.215(3) 1 calc PR A 2 C9B C 0.710(3) 0.341(3) 0.2311(15) 0.098(5) Uani 0.215(3) 1 d PDU A 2 H9BA H 0.6252 0.3257 0.2082 0.147 Uiso 0.215(3) 1 calc PR A 2 H9BB H 0.6844 0.4092 0.2659 0.147 Uiso 0.215(3) 1 calc PR A 2 H9BC H 0.7460 0.2523 0.2511 0.147 Uiso 0.215(3) 1 calc PR A 2 C10B C 0.434(3) 0.410(3) 0.0880(19) 0.066(3) Uani 0.215(3) 1 d PDU A 2 H10A H 0.5175 0.3485 0.0860 0.080 Uiso 0.215(3) 1 calc PR A 2 C11B C 0.318(3) 0.405(3) 0.0483(17) 0.070(3) Uani 0.215(3) 1 d PDU A 2 H11A H 0.2972 0.3300 0.0223 0.084 Uiso 0.215(3) 1 calc PR A 2 C12B C 0.242(3) 0.536(2) 0.0557(15) 0.074(3) Uani 0.215(3) 1 d PDU A 2 H12A H 0.1575 0.5658 0.0351 0.089 Uiso 0.215(3) 1 calc PR A 2 C13B C 0.310(3) 0.616(2) 0.0989(12) 0.076(4) Uani 0.215(3) 1 d PDU A 2 C14B C 0.248(2) 0.7391(19) 0.1261(10) 0.073(4) Uani 0.215(3) 1 d PDU A 2 H14B H 0.1610 0.7799 0.1117 0.087 Uiso 0.215(3) 1 calc PR A 2 C15B C 0.235(3) 0.938(4) 0.2057(16) 0.098(4) Uani 0.215(3) 1 d PDU A 2 C16B C 0.346(3) 0.988(3) 0.2509(16) 0.109(5) Uani 0.215(3) 1 d PDU A 2 H16D H 0.3052 1.0716 0.2742 0.164 Uiso 0.215(3) 1 calc PR A 2 H16E H 0.4333 1.0110 0.2235 0.164 Uiso 0.215(3) 1 calc PR A 2 H16F H 0.3694 0.9136 0.2832 0.164 Uiso 0.215(3) 1 calc PR A 2 C17B C 0.196(4) 1.064(3) 0.1582(18) 0.109(6) Uani 0.215(3) 1 d PDU A 2 H17D H 0.1461 1.1403 0.1842 0.164 Uiso 0.215(3) 1 calc PR A 2 H17E H 0.1329 1.0343 0.1261 0.164 Uiso 0.215(3) 1 calc PR A 2 H17F H 0.2834 1.0970 0.1347 0.164 Uiso 0.215(3) 1 calc PR A 2 C18B C 0.094(3) 0.896(4) 0.2465(16) 0.115(6) Uani 0.215(3) 1 d PDU A 2 H18D H 0.0451 0.9784 0.2673 0.173 Uiso 0.215(3) 1 calc PR A 2 H18E H 0.1186 0.8254 0.2807 0.173 Uiso 0.215(3) 1 calc PR A 2 H18F H 0.0318 0.8562 0.2169 0.173 Uiso 0.215(3) 1 calc PR A 2 N5 N 0.5144(4) 0.6467(4) 0.31000(18) 0.0684(10) Uani 1 1 d . A . N1A N 0.3966(9) 0.5607(7) 0.1200(5) 0.064(2) Uani 0.785(3) 1 d PDU A 1 N2A N 0.6576(5) 0.4389(5) 0.1605(2) 0.0660(13) Uani 0.785(3) 1 d PDU A 1 N3A N 0.6828(8) 0.7912(8) 0.1225(6) 0.0574(18) Uani 0.785(3) 1 d PDU A 1 N4A N 0.4004(5) 0.8881(5) 0.1695(2) 0.0637(13) Uani 0.785(3) 1 d PDU A 1 N1B N 0.646(4) 0.826(4) 0.123(3) 0.058(5) Uani 0.215(3) 1 d PGDU A 2 N2B N 0.7667(17) 0.5526(16) 0.1623(8) 0.065(4) Uani 0.215(3) 1 d PDU A 2 N3B N 0.404(3) 0.523(2) 0.1307(17) 0.059(5) Uani 0.215(3) 1 d PDU A 2 N4B N 0.3110(18) 0.7990(18) 0.1718(8) 0.064(4) Uani 0.215(3) 1 d PDU A 2 Si1 Si 0.40401(18) 0.52533(17) 0.34905(7) 0.0862(5) Uani 1 1 d . A . Si2 Si 0.6153(2) 0.75646(19) 0.35055(8) 0.0974(5) Uani 1 1 d . A . Y1 Y 0.52977(4) 0.66116(4) 0.19654(2) 0.05290(17) Uani 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 C19 0.175(7) 0.135(6) 0.104(5) 0.013(4) -0.011(5) -0.086(5) C20 0.177(7) 0.127(6) 0.121(6) 0.054(5) 0.005(5) -0.001(5) C21 0.141(6) 0.159(7) 0.116(5) -0.010(5) 0.046(5) -0.010(5) C22 0.183(7) 0.154(6) 0.097(5) -0.012(4) -0.023(5) -0.091(6) C23 0.201(8) 0.193(8) 0.139(7) 0.004(6) -0.106(6) -0.024(7) C24 0.230(9) 0.142(7) 0.116(6) -0.051(5) -0.007(6) -0.038(6) C1A 0.072(4) 0.091(4) 0.073(4) -0.024(3) -0.011(3) -0.011(3) C2A 0.076(3) 0.091(5) 0.068(4) -0.018(3) -0.015(3) -0.020(3) C3A 0.075(4) 0.081(4) 0.070(3) -0.019(3) -0.001(3) -0.021(3) C4A 0.063(4) 0.069(4) 0.059(4) -0.010(3) 0.000(3) -0.015(3) C5A 0.076(4) 0.062(3) 0.069(4) -0.010(3) 0.007(3) -0.003(3) C6A 0.074(5) 0.077(5) 0.102(4) 0.011(4) -0.012(4) 0.020(4) C7A 0.087(7) 0.110(8) 0.118(6) 0.017(6) 0.009(5) 0.046(5) C8A 0.109(5) 0.088(5) 0.127(6) 0.034(5) -0.004(5) 0.014(4) C9A 0.079(5) 0.108(5) 0.138(6) 0.005(4) -0.036(5) 0.009(4) C10A 0.065(4) 0.066(4) 0.069(5) 0.000(3) -0.001(3) -0.021(3) C11A 0.084(3) 0.072(4) 0.065(4) 0.007(3) -0.003(3) -0.022(3) C12A 0.106(4) 0.066(3) 0.069(3) 0.001(3) -0.008(4) -0.015(3) C13A 0.090(4) 0.046(4) 0.064(4) 0.003(3) -0.008(3) -0.005(3) C14A 0.095(4) 0.045(3) 0.064(4) 0.001(3) -0.008(3) 0.006(3) C15A 0.089(4) 0.080(4) 0.087(4) -0.008(3) 0.003(4) 0.034(3) C16A 0.086(5) 0.114(6) 0.110(5) 0.003(4) 0.016(5) 0.025(4) C17A 0.112(6) 0.109(6) 0.126(6) -0.001(5) -0.030(4) 0.049(5) C18A 0.148(7) 0.116(6) 0.130(6) -0.056(5) 0.013(5) 0.023(5) C1B 0.092(5) 0.053(6) 0.065(5) 0.003(5) -0.006(5) -0.010(5) C2B 0.092(5) 0.059(5) 0.065(5) 0.005(5) -0.004(5) -0.019(5) C3B 0.076(5) 0.062(6) 0.064(6) 0.007(5) -0.002(5) -0.023(5) C4B 0.073(7) 0.058(6) 0.064(7) 0.006(5) -0.006(6) -0.028(6) C5B 0.061(7) 0.061(6) 0.066(8) -0.001(6) -0.007(7) -0.021(6) C6B 0.072(7) 0.086(7) 0.107(7) 0.017(7) -0.015(6) 0.025(7) C7B 0.072(11) 0.095(12) 0.107(9) 0.016(10) -0.016(8) 0.043(10) C8B 0.084(10) 0.109(13) 0.122(11) 0.015(11) -0.033(10) 0.018(10) C9B 0.105(10) 0.066(10) 0.119(10) 0.029(10) -0.003(8) 0.008(9) C10B 0.067(5) 0.071(5) 0.064(5) -0.019(5) -0.001(5) -0.013(5) C11B 0.069(5) 0.080(5) 0.065(5) -0.020(5) -0.007(5) -0.017(5) C12B 0.070(5) 0.086(6) 0.070(6) -0.021(5) -0.011(5) -0.017(5) C13B 0.070(7) 0.088(7) 0.073(7) -0.022(6) -0.006(6) -0.021(6) C14B 0.062(7) 0.089(7) 0.071(7) -0.021(6) -0.012(7) -0.009(7) C15B 0.095(7) 0.092(7) 0.101(7) -0.009(6) 0.000(6) 0.036(6) C16B 0.115(10) 0.091(11) 0.118(10) -0.016(10) -0.016(8) 0.035(9) C17B 0.110(11) 0.096(11) 0.116(11) 0.001(9) -0.010(9) 0.038(10) C18B 0.097(10) 0.123(13) 0.115(12) 0.002(11) 0.013(11) 0.038(10) N5 0.082(3) 0.070(2) 0.053(2) -0.0014(19) -0.009(2) -0.004(2) N1A 0.073(3) 0.061(4) 0.059(4) -0.005(4) -0.008(3) -0.007(3) N2A 0.060(3) 0.062(3) 0.074(3) 0.003(3) -0.004(3) 0.002(2) N3A 0.048(5) 0.058(4) 0.064(3) -0.002(4) -0.001(4) 0.002(3) N4A 0.071(3) 0.055(3) 0.063(3) -0.002(3) -0.006(3) 0.009(2) N1B 0.038(10) 0.066(11) 0.066(8) -0.001(10) -0.003(9) 0.012(8) N2B 0.067(8) 0.056(7) 0.071(8) -0.010(7) -0.007(7) 0.017(7) N3B 0.077(8) 0.050(10) 0.053(9) 0.002(9) -0.006(7) -0.017(8) N4B 0.063(8) 0.070(8) 0.054(7) 0.013(7) -0.007(7) 0.023(7) Si1 0.1064(12) 0.0885(11) 0.0620(9) 0.0057(8) 0.0034(8) -0.0131(9) Si2 0.1305(14) 0.1037(13) 0.0642(10) -0.0087(9) -0.0243(10) -0.0269(11) Y1 0.0582(3) 0.0501(3) 0.0507(3) -0.00270(18) -0.00630(18) -0.00341(18) _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 C19 Si1 1.860(6) . ? C20 Si1 1.873(6) . ? C21 Si1 1.860(6) . ? C22 Si2 1.845(6) . ? C23 Si2 1.877(7) . ? C24 Si2 1.879(7) . ? C1A N1A 1.360(6) . ? C1A C2A 1.400(6) . ? C2A C3A 1.393(6) . ? C3A C4A 1.407(6) . ? C4A N1A 1.366(6) . ? C4A C5A 1.378(7) . ? C5A N2A 1.282(6) . ? C6A N2A 1.493(11) . ? C6A C9A 1.525(7) . ? C6A C8A 1.529(7) . ? C6A C7A 1.533(7) . ? C10A N3A 1.366(5) . ? C10A C11A 1.384(7) . ? C11A C12A 1.388(7) . ? C12A C13A 1.391(7) . ? C13A N3A 1.368(6) . ? C13A C14A 1.391(7) . ? C14A N4A 1.288(6) . ? C15A N4A 1.495(11) . ? C15A C16A 1.521(7) . ? C15A C18A 1.527(7) . ? C15A C17A 1.533(7) . ? C1B C2B 1.4200 . ? C1B N1B 1.382(8) . ? C2B C3B 1.4200 . ? C3B C4B 1.4200 . ? C4B C5B 1.366(10) . ? C4B N1B 1.381(8) . ? C4B Y1 2.99(3) . ? C5B N2B 1.283(9) . ? C6B C9B 1.530(9) . ? C6B C8B 1.531(9) . ? C6B C7B 1.532(9) . ? C6B N2B 1.56(5) . ? C10B N3B 1.371(8) . ? C10B C11B 1.384(9) . ? C11B C12B 1.379(9) . ? C12B C13B 1.379(9) . ? C13B C14B 1.362(10) . ? C13B N3B 1.364(8) . ? C14B N4B 1.283(9) . ? C15B C16B 1.529(9) . ? C15B C17B 1.530(9) . ? C15B C18B 1.531(9) . ? C15B N4B 1.58(4) . ? N5 Si1 1.699(4) . ? N5 Si2 1.703(4) . ? N5 Y1 2.245(4) . ? N1A Y1 2.303(4) . ? N2A Y1 2.420(5) . ? N3A Y1 2.318(4) . ? N4A Y1 2.433(4) . ? N1B Y1 2.331(8) . ? N2B Y1 2.392(15) . ? N3B Y1 2.312(8) . ? N4B Y1 2.395(15) . ? Si1 Y1 3.3829(15) . ? Si2 Y1 3.3915(16) . ? 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 N1A C1A C2A 111.0(6) . . ? C3A C2A C1A 106.9(6) . . ? C2A C3A C4A 105.0(5) . . ? N1A C4A C5A 119.8(6) . . ? N1A C4A C3A 111.6(5) . . ? C5A C4A C3A 128.5(6) . . ? N2A C5A C4A 123.2(6) . . ? N2A C6A C9A 106.0(7) . . ? N2A C6A C8A 109.2(6) . . ? C9A C6A C8A 108.0(7) . . ? N2A C6A C7A 112.6(8) . . ? C9A C6A C7A 113.8(10) . . ? C8A C6A C7A 107.1(9) . . ? N3A C10A C11A 112.3(5) . . ? C10A C11A C12A 104.7(5) . . ? C11A C12A C13A 108.1(5) . . ? N3A C13A C14A 120.6(6) . . ? N3A C13A C12A 109.7(4) . . ? C14A C13A C12A 129.7(6) . . ? N4A C14A C13A 122.5(5) . . ? N4A C15A C16A 108.5(6) . . ? N4A C15A C18A 107.8(6) . . ? C16A C15A C18A 110.7(7) . . ? N4A C15A C17A 110.2(6) . . ? C16A C15A C17A 110.1(7) . . ? C18A C15A C17A 109.4(7) . . ? C2B C1B N1B 105.7(4) . . ? C3B C2B C1B 108.0 . . ? C2B C3B C4B 108.0 . . ? C5B C4B N1B 133(3) . . ? C5B C4B C3B 121(2) . . ? N1B C4B C3B 105.7(4) . . ? C5B C4B Y1 84.0(15) . . ? N1B C4B Y1 49.0(12) . . ? C3B C4B Y1 154.5(12) . . ? N2B C5B C4B 113.9(19) . . ? C9B C6B C8B 108(2) . . ? C9B C6B C7B 131(4) . . ? C8B C6B C7B 109(4) . . ? C9B C6B N2B 104(3) . . ? C8B C6B N2B 103(3) . . ? C7B C6B N2B 98(3) . . ? N3B C10B C11B 108.4(12) . . ? C12B C11B C10B 104.8(10) . . ? C13B C12B C11B 108.7(7) . . ? C14B C13B N3B 124.1(13) . . ? C14B C13B C12B 123.1(19) . . ? N3B C13B C12B 106.4(10) . . ? N4B C14B C13B 119.6(16) . . ? C16B C15B C17B 107(3) . . ? C16B C15B C18B 112(3) . . ? C17B C15B C18B 108(3) . . ? C16B C15B N4B 105(2) . . ? C17B C15B N4B 117(3) . . ? C18B C15B N4B 108(2) . . ? Si1 N5 Si2 124.8(2) . . ? Si1 N5 Y1 117.45(19) . . ? Si2 N5 Y1 117.76(19) . . ? C1A N1A C4A 105.2(5) . . ? C1A N1A Y1 140.7(5) . . ? C4A N1A Y1 114.1(4) . . ? C5A N2A C6A 119.4(5) . . ? C5A N2A Y1 111.4(4) . . ? C6A N2A Y1 129.2(4) . . ? C10A N3A C13A 105.2(5) . . ? C10A N3A Y1 140.9(5) . . ? C13A N3A Y1 113.1(4) . . ? C14A N4A C15A 119.5(5) . . ? C14A N4A Y1 111.2(4) . . ? C15A N4A Y1 129.2(4) . . ? C4B N1B C1B 112.5(7) . . ? C4B N1B Y1 104.4(17) . . ? C1B N1B Y1 142.8(18) . . ? C5B N2B C6B 117.3(15) . . ? C5B N2B Y1 114.9(12) . . ? C6B N2B Y1 127.5(12) . . ? C13B N3B C10B 105.3(10) . . ? C13B N3B Y1 105.6(12) . . ? C10B N3B Y1 138(2) . . ? C14B N4B C15B 119.4(16) . . ? C14B N4B Y1 110.3(13) . . ? C15B N4B Y1 130.1(13) . . ? N5 Si1 C19 108.6(2) . . ? N5 Si1 C21 114.5(3) . . ? C19 Si1 C21 106.6(3) . . ? N5 Si1 C20 114.6(3) . . ? C19 Si1 C20 105.8(3) . . ? C21 Si1 C20 106.2(3) . . ? N5 Si1 Y1 36.09(12) . . ? C19 Si1 Y1 72.50(18) . . ? C21 Si1 Y1 127.5(2) . . ? C20 Si1 Y1 124.9(2) . . ? N5 Si2 C22 109.2(2) . . ? N5 Si2 C23 113.6(3) . . ? C22 Si2 C23 106.1(4) . . ? N5 Si2 C24 114.0(3) . . ? C22 Si2 C24 107.1(3) . . ? C23 Si2 C24 106.3(4) . . ? N5 Si2 Y1 35.86(12) . . ? C22 Si2 Y1 73.36(19) . . ? C23 Si2 Y1 124.7(3) . . ? C24 Si2 Y1 127.2(3) . . ? N5 Y1 N1B 129.2(16) . . ? N5 Y1 N1A 131.1(3) . . ? N1B Y1 N1A 98.2(17) . . ? N5 Y1 N3B 124.0(10) . . ? N1B Y1 N3B 106.5(19) . . ? N1A Y1 N3B 10.3(8) . . ? N5 Y1 N3A 129.3(4) . . ? N1B Y1 N3A 11.2(7) . . ? N1A Y1 N3A 99.5(5) . . ? N3B Y1 N3A 106.5(11) . . ? N5 Y1 N2B 104.4(4) . . ? N1B Y1 N2B 73.7(8) . . ? N1A Y1 N2B 99.2(5) . . ? N3B Y1 N2B 95.5(9) . . ? N3A Y1 N2B 62.5(4) . . ? N5 Y1 N4B 103.9(4) . . ? N1B Y1 N4B 84.1(9) . . ? N1A Y1 N4B 65.4(4) . . ? N3B Y1 N4B 73.0(7) . . ? N3A Y1 N4B 94.7(5) . . ? N2B Y1 N4B 151.1(6) . . ? N5 Y1 N2A 104.92(15) . . ? N1B Y1 N2A 101.3(9) . . ? N1A Y1 N2A 71.5(2) . . ? N3B Y1 N2A 64.4(6) . . ? N3A Y1 N2A 91.1(2) . . ? N2B Y1 N2A 36.8(4) . . ? N4B Y1 N2A 136.9(4) . . ? N5 Y1 N4A 104.95(14) . . ? N1B Y1 N4A 60.4(7) . . ? N1A Y1 N4A 87.0(2) . . ? N3B Y1 N4A 96.4(5) . . ? N3A Y1 N4A 71.62(18) . . ? N2B Y1 N4A 134.1(4) . . ? N4B Y1 N4A 29.0(4) . . ? N2A Y1 N4A 150.03(17) . . ? N5 Y1 C4B 126.9(7) . . ? N1B Y1 C4B 26.6(5) . . ? N1A Y1 C4B 100.4(8) . . ? N3B Y1 C4B 105.0(13) . . ? N3A Y1 C4B 15.4(3) . . ? N2B Y1 C4B 47.1(4) . . ? N4B Y1 C4B 109.2(6) . . ? N2A Y1 C4B 77.0(4) . . ? N4A Y1 C4B 87.0(3) . . ? N5 Y1 Si1 26.47(10) . . ? N1B Y1 Si1 155.3(16) . . ? N1A Y1 Si1 105.0(3) . . ? N3B Y1 Si1 97.5(10) . . ? N3A Y1 Si1 155.4(4) . . ? N2B Y1 Si1 110.3(4) . . ? N4B Y1 Si1 97.6(4) . . ? N2A Y1 Si1 94.21(11) . . ? N4A Y1 Si1 111.78(12) . . ? C4B Y1 Si1 148.9(6) . . ? N5 Y1 Si2 26.38(10) . . ? N1B Y1 Si2 103.0(16) . . ? N1A Y1 Si2 156.9(3) . . ? N3B Y1 Si2 150.3(10) . . ? N3A Y1 Si2 103.1(4) . . ? N2B Y1 Si2 95.5(4) . . ? N4B Y1 Si2 107.6(4) . . ? N2A Y1 Si2 112.51(12) . . ? N4A Y1 Si2 95.52(12) . . ? C4B Y1 Si2 102.7(8) . . ? Si1 Y1 Si2 52.84(4) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.316 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.058 data_3b _database_code_depnum_ccdc_archive 'CCDC 896987' #TrackingRef 'CCDC 896987.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H44 Dy N5 Si2' _chemical_formula_weight 621.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2378(9) _cell_length_b 9.3434(9) _cell_length_c 19.929(2) _cell_angle_alpha 87.8880(10) _cell_angle_beta 84.6720(10) _cell_angle_gamma 86.2540(10) _cell_volume 1708.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9921 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.53 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 634 _exptl_absorpt_coefficient_mu 2.274 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5391 _exptl_absorpt_correction_T_max 0.6719 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13010 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6605 _reflns_number_gt 6010 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Some highly disordered solvent peaks of solvent molecule were observed but could not be modelled satisfactorily. The SQUEEZE routine in PLATON was used to modify the HKL file. Restraints have been applied to refine the ligand which is affected by disorder. sadi 0.01 c5a n2a c5b n2b c14a n4a c14b n4b sadi 0.01 c15A c16a c15B c16b c15A c17a c15B c17b c15A c18a c15B c18b sadi 0.01 c6A c7a c6A c8a c6A c9a c6B c7b c6B c8b c6B c9b SADI 0.01 C13B C14B C13A C14A C4A C5A C4B C5B sadi 0.01 c10a c11a c10b c11b c11a c12a c11b c12b c12a c13a c12b c13b sadi 0.01 c1a c2a c2a c3a c3a c4a c1b c2b c2b c3b c3b c4b sadi 0.01 n1a c4a n1a c1a n1b c4b n1b c1b n3a c13a n3a c10a n3b c13b n3b c10b sadi 0.01 n3a c14a n3b c14b sadi 0.01 c10a c12a c10b c12b c10a c13a c10b c13b DELU 0.01 $C DELU 0.01 $N SIMU 0.01 $C SIMU 0.01 $N ; _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^)+(0.0576P)^2^+1.3981P] 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 6605 _refine_ls_number_parameters 496 _refine_ls_number_restraints 579 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.932 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.496 0.500 268 45 ' ' 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 Dy1 Dy 0.529071(18) 0.163134(17) 0.197445(8) 0.04882(8) Uani 1 1 d . . . Si1 Si 0.40302(19) 0.02568(17) 0.34944(7) 0.0812(4) Uani 1 1 d . A . Si2 Si 0.6173(2) 0.2571(2) 0.35083(7) 0.0915(5) Uani 1 1 d . A . N5 N 0.5140(4) 0.1472(4) 0.30975(17) 0.0639(8) Uani 1 1 d . A . C19 C 0.3175(9) -0.0660(8) 0.2845(3) 0.132(3) Uani 1 1 d . . . H19A H 0.2488 -0.0002 0.2643 0.198 Uiso 1 1 calc R A . H19B H 0.2681 -0.1461 0.3048 0.198 Uiso 1 1 calc R . . H19C H 0.3912 -0.0994 0.2505 0.198 Uiso 1 1 calc R . . C20 C 0.2535(9) 0.1006(9) 0.4094(4) 0.132(3) Uani 1 1 d . . . H20A H 0.2888 0.1754 0.4340 0.198 Uiso 1 1 calc R A . H20B H 0.2200 0.0260 0.4402 0.198 Uiso 1 1 calc R . . H20C H 0.1745 0.1392 0.3848 0.198 Uiso 1 1 calc R . . C21 C 0.4942(11) -0.1245(9) 0.3962(4) 0.149(3) Uani 1 1 d . . . H21A H 0.4861 -0.2126 0.3739 0.224 Uiso 1 1 calc R A . H21B H 0.4485 -0.1314 0.4413 0.224 Uiso 1 1 calc R . . H21C H 0.5952 -0.1072 0.3974 0.224 Uiso 1 1 calc R . . C22 C 0.7148(9) 0.3731(9) 0.2859(3) 0.131(3) Uani 1 1 d . . . H22A H 0.7811 0.3144 0.2570 0.196 Uiso 1 1 calc R A . H22B H 0.7680 0.4400 0.3077 0.196 Uiso 1 1 calc R . . H22C H 0.6454 0.4246 0.2595 0.196 Uiso 1 1 calc R . . C23 C 0.5090(13) 0.3812(10) 0.4104(4) 0.172(4) Uani 1 1 d . . . H23A H 0.4665 0.4605 0.3855 0.258 Uiso 1 1 calc R A . H23B H 0.5717 0.4162 0.4411 0.258 Uiso 1 1 calc R . . H23C H 0.4332 0.3306 0.4353 0.258 Uiso 1 1 calc R . . C24 C 0.7573(11) 0.1585(11) 0.3992(5) 0.170(4) Uani 1 1 d . . . H24A H 0.8466 0.2063 0.3926 0.255 Uiso 1 1 calc R A . H24B H 0.7736 0.0622 0.3837 0.255 Uiso 1 1 calc R . . H24C H 0.7238 0.1560 0.4463 0.255 Uiso 1 1 calc R . . N1A N 0.3915(12) 0.0566(14) 0.1229(9) 0.061(2) Uani 0.717(3) 1 d PDU A 1 N2A N 0.6590(5) -0.0601(5) 0.1606(2) 0.0590(11) Uani 0.717(3) 1 d PDU A 1 N3A N 0.6834(9) 0.3001(12) 0.1245(7) 0.057(2) Uani 0.717(3) 1 d PDU A 1 N4A N 0.3978(5) 0.3914(5) 0.1700(2) 0.0586(11) Uani 0.717(3) 1 d PDU A 1 C1A C 0.2679(9) 0.0775(9) 0.0902(5) 0.0729(18) Uani 0.717(3) 1 d PDU A 1 H1A H 0.1995 0.1541 0.0978 0.087 Uiso 0.717(3) 1 calc PR A 1 C2A C 0.2560(8) -0.0282(8) 0.0446(4) 0.0702(16) Uani 0.717(3) 1 d PDU A 1 H2A H 0.1817 -0.0347 0.0166 0.084 Uiso 0.717(3) 1 calc PR A 1 C3A C 0.3765(8) -0.1219(8) 0.0490(4) 0.0663(16) Uani 0.717(3) 1 d PDU A 1 H3A H 0.3995 -0.2046 0.0246 0.080 Uiso 0.717(3) 1 calc PR A 1 C4A C 0.4571(9) -0.0686(10) 0.0970(5) 0.0611(16) Uani 0.717(3) 1 d PDU A 1 C5A C 0.5915(6) -0.1219(6) 0.1172(3) 0.0608(13) Uani 0.717(3) 1 d PDU A 1 H5A H 0.6341 -0.2059 0.0985 0.073 Uiso 0.717(3) 1 calc PR A 1 C6A C 0.7970(9) -0.1270(8) 0.1798(4) 0.0739(18) Uani 0.717(3) 1 d PDU A 1 C7A C 0.9079(10) -0.1533(13) 0.1200(6) 0.094(3) Uani 0.717(3) 1 d PDU A 1 H7A H 0.8767 -0.2270 0.0933 0.141 Uiso 0.717(3) 1 calc PR A 1 H7B H 1.0006 -0.1831 0.1356 0.141 Uiso 0.717(3) 1 calc PR A 1 H7C H 0.9165 -0.0664 0.0930 0.141 Uiso 0.717(3) 1 calc PR A 1 C8A C 0.7722(10) -0.2672(8) 0.2193(5) 0.099(2) Uani 0.717(3) 1 d PDU A 1 H8A H 0.8624 -0.3055 0.2351 0.149 Uiso 0.717(3) 1 calc PR A 1 H8B H 0.7367 -0.3348 0.1907 0.149 Uiso 0.717(3) 1 calc PR A 1 H8C H 0.7019 -0.2498 0.2572 0.149 Uiso 0.717(3) 1 calc PR A 1 C9A C 0.8574(9) -0.0263(9) 0.2267(5) 0.098(2) Uani 0.717(3) 1 d PDU A 1 H9A H 0.9494 -0.0663 0.2397 0.147 Uiso 0.717(3) 1 calc PR A 1 H9B H 0.7905 -0.0137 0.2662 0.147 Uiso 0.717(3) 1 calc PR A 1 H9C H 0.8705 0.0649 0.2039 0.147 Uiso 0.717(3) 1 calc PR A 1 C10A C 0.8133(11) 0.2823(11) 0.0864(6) 0.0676(19) Uani 0.717(3) 1 d PDU A 1 H10A H 0.8806 0.2049 0.0908 0.081 Uiso 0.717(3) 1 calc PR A 1 C11A C 0.8309(10) 0.3950(9) 0.0406(5) 0.0717(18) Uani 0.717(3) 1 d PDU A 1 H11A H 0.9132 0.4110 0.0113 0.086 Uiso 0.717(3) 1 calc PR A 1 C12A C 0.7032(7) 0.4793(8) 0.0465(4) 0.0688(16) Uani 0.717(3) 1 d PDU A 1 H12A H 0.6825 0.5629 0.0215 0.083 Uiso 0.717(3) 1 calc PR A 1 C14A C 0.4700(7) 0.4622(6) 0.1230(3) 0.0635(14) Uani 0.717(3) 1 d PDU A 1 H14A H 0.4268 0.5469 0.1059 0.076 Uiso 0.717(3) 1 calc PR A 1 C13A C 0.6107(7) 0.4176(7) 0.0964(5) 0.0629(16) Uani 0.717(3) 1 d PDU A 1 C15A C 0.2489(12) 0.4511(9) 0.1970(4) 0.0827(19) Uani 0.717(3) 1 d PDU A 1 C16A C 0.1857(9) 0.3359(9) 0.2429(5) 0.099(2) Uani 0.717(3) 1 d PDU A 1 H16A H 0.0820 0.3541 0.2502 0.148 Uiso 0.717(3) 1 calc PR A 1 H16B H 0.2274 0.3354 0.2853 0.148 Uiso 0.717(3) 1 calc PR A 1 H16C H 0.2072 0.2443 0.2227 0.148 Uiso 0.717(3) 1 calc PR A 1 C17A C 0.1582(13) 0.4935(12) 0.1397(5) 0.111(3) Uani 0.717(3) 1 d PDU A 1 H17A H 0.1193 0.5907 0.1448 0.167 Uiso 0.717(3) 1 calc PR A 1 H17B H 0.0796 0.4310 0.1402 0.167 Uiso 0.717(3) 1 calc PR A 1 H17C H 0.2178 0.4859 0.0978 0.167 Uiso 0.717(3) 1 calc PR A 1 C18A C 0.2668(12) 0.5799(10) 0.2375(5) 0.116(3) Uani 0.717(3) 1 d PDU A 1 H18A H 0.1734 0.6152 0.2575 0.174 Uiso 0.717(3) 1 calc PR A 1 H18B H 0.3091 0.6535 0.2085 0.174 Uiso 0.717(3) 1 calc PR A 1 H18C H 0.3295 0.5535 0.2723 0.174 Uiso 0.717(3) 1 calc PR A 1 N1B N 0.649(3) 0.311(3) 0.117(2) 0.056(4) Uani 0.283(3) 1 d PDU A 2 N2B N 0.7695(12) 0.0516(11) 0.1592(6) 0.054(2) Uani 0.283(3) 1 d PDU A 2 N3B N 0.424(4) 0.040(4) 0.119(2) 0.066(5) Uani 0.283(3) 1 d PDU A 2 N4B N 0.3047(13) 0.2956(13) 0.1737(6) 0.063(3) Uani 0.283(3) 1 d PDU A 2 C1B C 0.643(2) 0.448(2) 0.0903(14) 0.066(3) Uani 0.283(3) 1 d PDU A 2 H1B H 0.5680 0.5164 0.1019 0.079 Uiso 0.283(3) 1 calc PR A 2 C2B C 0.761(2) 0.475(2) 0.0445(12) 0.067(3) Uani 0.283(3) 1 d PDU A 2 H2B H 0.7729 0.5565 0.0166 0.081 Uiso 0.283(3) 1 calc PR A 2 C3B C 0.857(3) 0.356(2) 0.0488(14) 0.067(3) Uani 0.283(3) 1 d PDU A 2 H3B H 0.9460 0.3384 0.0236 0.080 Uiso 0.283(3) 1 calc PR A 2 C4B C 0.792(3) 0.269(2) 0.0990(18) 0.065(3) Uani 0.283(3) 1 d PDU A 2 C5B C 0.8459(15) 0.1310(15) 0.1172(7) 0.065(3) Uani 0.283(3) 1 d PDU A 2 H5B H 0.9372 0.0963 0.0989 0.078 Uiso 0.283(3) 1 calc PR A 2 C6B C 0.8375(16) -0.103(3) 0.1788(9) 0.077(3) Uani 0.283(3) 1 d PDU A 2 C7B C 0.8796(17) -0.189(3) 0.1159(13) 0.081(5) Uani 0.283(3) 1 d PDU A 2 H7D H 0.9097 -0.2858 0.1288 0.121 Uiso 0.283(3) 1 calc PR A 2 H7E H 0.9584 -0.1461 0.0894 0.121 Uiso 0.283(3) 1 calc PR A 2 H7F H 0.7974 -0.1900 0.0899 0.121 Uiso 0.283(3) 1 calc PR A 2 C8B C 0.9663(18) -0.076(2) 0.2180(9) 0.096(4) Uani 0.283(3) 1 d PRDU A 2 H8D H 1.0067 -0.1683 0.2359 0.144 Uiso 0.283(3) 1 d PR A 2 H8E H 0.9334 -0.0165 0.2553 0.144 Uiso 0.283(3) 1 d PR A 2 H8F H 1.0369 -0.0301 0.1908 0.144 Uiso 0.283(3) 1 d PR A 2 C9B C 0.721(2) -0.167(2) 0.2277(12) 0.094(4) Uani 0.283(3) 1 d PDU A 2 H9D H 0.7213 -0.2682 0.2212 0.140 Uiso 0.283(3) 1 calc PR A 2 H9E H 0.6274 -0.1224 0.2195 0.140 Uiso 0.283(3) 1 calc PR A 2 H9F H 0.7409 -0.1503 0.2731 0.140 Uiso 0.283(3) 1 calc PR A 2 C10B C 0.442(3) -0.085(2) 0.0843(14) 0.062(3) Uani 0.283(3) 1 d PDU A 2 H10B H 0.5176 -0.1552 0.0886 0.075 Uiso 0.283(3) 1 calc PR A 2 C11B C 0.333(2) -0.093(2) 0.0426(12) 0.066(2) Uani 0.283(3) 1 d PDU A 2 H11B H 0.3203 -0.1670 0.0141 0.080 Uiso 0.283(3) 1 calc PR A 2 C12B C 0.2447(19) 0.0307(18) 0.0514(11) 0.069(3) Uani 0.283(3) 1 d PDU A 2 H12B H 0.1632 0.0570 0.0286 0.083 Uiso 0.283(3) 1 calc PR A 2 C13B C 0.298(2) 0.109(2) 0.0997(13) 0.071(3) Uani 0.283(3) 1 d PDU A 2 C14B C 0.2433(15) 0.2384(15) 0.1269(7) 0.069(3) Uani 0.283(3) 1 d PDU A 2 H14B H 0.1605 0.2846 0.1110 0.083 Uiso 0.283(3) 1 calc PR A 2 C15B C 0.241(3) 0.432(3) 0.2020(11) 0.091(3) Uani 0.283(3) 1 d PDU A 2 C16B C 0.338(2) 0.489(2) 0.2498(12) 0.098(4) Uani 0.283(3) 1 d PDU A 2 H16D H 0.2817 0.5159 0.2907 0.147 Uiso 0.283(3) 1 calc PR A 2 H16E H 0.3842 0.5710 0.2293 0.147 Uiso 0.283(3) 1 calc PR A 2 H16F H 0.4118 0.4156 0.2598 0.147 Uiso 0.283(3) 1 calc PR A 2 C17B C 0.198(3) 0.554(3) 0.1556(15) 0.104(5) Uani 0.283(3) 1 d PDU A 2 H17D H 0.2403 0.5363 0.1107 0.156 Uiso 0.283(3) 1 calc PR A 2 H17E H 0.2320 0.6417 0.1705 0.156 Uiso 0.283(3) 1 calc PR A 2 H17F H 0.0937 0.5635 0.1559 0.156 Uiso 0.283(3) 1 calc PR A 2 C18B C 0.109(3) 0.398(3) 0.2483(14) 0.109(5) Uani 0.283(3) 1 d PDU A 2 H18D H 0.1116 0.4442 0.2903 0.163 Uiso 0.283(3) 1 calc PR A 2 H18E H 0.1090 0.2958 0.2563 0.163 Uiso 0.283(3) 1 calc PR A 2 H18F H 0.0226 0.4311 0.2277 0.163 Uiso 0.283(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.05069(11) 0.04561(11) 0.05063(11) -0.00203(7) -0.00712(7) -0.00261(7) Si1 0.0999(10) 0.0836(9) 0.0583(7) 0.0079(6) 0.0034(7) -0.0133(8) Si2 0.1192(13) 0.1016(11) 0.0595(8) -0.0090(7) -0.0232(8) -0.0263(10) N5 0.073(2) 0.063(2) 0.0563(19) 0.0016(15) -0.0110(16) -0.0027(17) C19 0.173(7) 0.142(6) 0.089(4) 0.004(4) 0.001(4) -0.098(6) C20 0.138(6) 0.147(7) 0.102(5) 0.000(4) 0.039(5) -0.006(5) C21 0.195(9) 0.125(6) 0.119(6) 0.049(5) 0.005(6) -0.007(6) C22 0.160(7) 0.147(6) 0.098(5) -0.005(4) -0.025(4) -0.096(6) C23 0.264(13) 0.138(7) 0.115(6) -0.068(6) 0.004(7) -0.019(8) C24 0.183(9) 0.193(10) 0.155(8) 0.011(7) -0.118(7) -0.038(7) N1A 0.054(5) 0.068(4) 0.061(4) -0.013(3) -0.004(5) -0.004(3) N2A 0.057(3) 0.050(2) 0.068(3) 0.003(2) -0.002(2) -0.0010(19) N3A 0.053(5) 0.065(3) 0.057(4) 0.008(2) -0.014(4) -0.016(3) N4A 0.066(3) 0.049(2) 0.059(3) -0.004(2) -0.008(2) 0.008(2) C1A 0.064(4) 0.087(4) 0.070(4) -0.020(3) -0.012(3) -0.006(3) C2A 0.069(3) 0.081(4) 0.065(3) -0.016(3) -0.013(3) -0.020(3) C3A 0.074(4) 0.068(3) 0.060(3) -0.011(3) -0.008(3) -0.017(3) C4A 0.064(3) 0.065(3) 0.057(4) -0.008(3) -0.005(2) -0.019(3) C5A 0.068(3) 0.052(3) 0.062(3) -0.008(2) 0.003(2) -0.002(2) C6A 0.060(4) 0.064(4) 0.093(4) 0.010(3) -0.002(3) 0.014(3) C7A 0.071(5) 0.087(8) 0.116(5) 0.009(4) 0.008(4) 0.018(5) C8A 0.095(5) 0.079(4) 0.117(6) 0.031(4) -0.006(4) 0.019(4) C9A 0.070(4) 0.105(5) 0.121(6) -0.001(4) -0.034(4) 0.015(4) C10A 0.063(4) 0.073(3) 0.068(5) -0.003(3) -0.006(3) -0.011(3) C11A 0.073(4) 0.072(4) 0.071(3) 0.002(3) 0.002(3) -0.024(3) C12A 0.080(4) 0.060(3) 0.067(3) 0.002(2) -0.002(4) -0.018(3) C14A 0.081(3) 0.045(3) 0.063(3) -0.001(2) -0.008(3) 0.006(2) C13A 0.075(4) 0.053(4) 0.062(3) -0.004(3) -0.006(3) -0.014(3) C15A 0.077(4) 0.077(4) 0.089(4) -0.007(3) -0.003(3) 0.032(3) C16A 0.072(4) 0.101(5) 0.114(6) 0.003(4) 0.014(4) 0.027(4) C17A 0.105(7) 0.111(7) 0.113(6) -0.011(5) -0.025(4) 0.052(5) C18A 0.123(6) 0.092(5) 0.127(6) -0.039(5) 0.007(5) 0.032(5) N1B 0.046(9) 0.071(8) 0.056(8) -0.004(6) -0.018(8) -0.022(6) N2B 0.048(5) 0.049(5) 0.064(6) 0.005(4) -0.005(4) 0.002(4) N3B 0.065(11) 0.075(8) 0.059(7) -0.017(7) -0.003(10) -0.011(7) N4B 0.062(6) 0.059(6) 0.065(6) 0.003(5) 0.001(5) 0.010(5) C1B 0.075(5) 0.055(5) 0.066(5) -0.001(5) 0.000(5) -0.004(5) C2B 0.070(6) 0.062(5) 0.070(5) -0.001(4) 0.001(5) -0.018(5) C3B 0.065(5) 0.069(5) 0.068(5) -0.001(5) 0.000(5) -0.016(4) C4B 0.064(5) 0.069(5) 0.064(6) 0.000(4) -0.002(5) -0.019(5) C5B 0.056(6) 0.074(5) 0.064(6) -0.011(5) -0.003(5) -0.001(5) C6B 0.061(6) 0.071(6) 0.095(6) 0.007(5) -0.013(5) 0.021(6) C7B 0.070(9) 0.062(10) 0.110(8) -0.008(7) -0.007(7) 0.002(8) C8B 0.081(8) 0.099(10) 0.109(10) -0.002(8) -0.031(8) 0.019(8) C9B 0.083(8) 0.074(8) 0.118(9) 0.014(8) 0.001(7) 0.016(7) C10B 0.066(5) 0.063(5) 0.060(5) -0.012(4) -0.005(4) -0.013(4) C11B 0.065(5) 0.075(5) 0.062(4) -0.010(4) -0.009(4) -0.019(4) C12B 0.063(5) 0.083(6) 0.065(5) -0.012(5) -0.012(4) -0.019(5) C13B 0.062(6) 0.087(6) 0.067(6) -0.018(5) -0.011(5) -0.020(6) C14B 0.052(6) 0.089(6) 0.067(6) -0.008(5) -0.010(5) -0.003(5) C15B 0.085(6) 0.084(6) 0.099(6) -0.008(5) -0.006(5) 0.036(6) C16B 0.100(8) 0.065(8) 0.128(9) -0.007(8) -0.013(7) 0.016(7) C17B 0.100(10) 0.087(10) 0.122(10) -0.001(8) -0.014(8) 0.025(9) C18B 0.090(8) 0.105(10) 0.125(10) -0.013(8) 0.008(8) 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 Dy1 N5 2.230(3) . ? Dy1 N3B 2.301(17) . ? Dy1 N1B 2.33(2) . ? Dy1 N1A 2.332(7) . ? Dy1 N3A 2.345(9) . ? Dy1 N4B 2.419(12) . ? Dy1 N2A 2.439(4) . ? Dy1 N4A 2.453(4) . ? Dy1 N2B 2.458(11) . ? Dy1 Si1 3.3815(13) . ? Dy1 Si2 3.3961(14) . ? Si1 N5 1.703(4) . ? Si1 C19 1.842(7) . ? Si1 C21 1.855(7) . ? Si1 C20 1.858(7) . ? Si2 N5 1.724(4) . ? Si2 C24 1.861(8) . ? Si2 C22 1.862(7) . ? Si2 C23 1.866(8) . ? N1A C1A 1.366(6) . ? N1A C4A 1.377(6) . ? N2A C5A 1.286(6) . ? N2A C6A 1.460(10) . ? N3A C10A 1.363(7) . ? N3A C13A 1.378(6) . ? N4A C14A 1.287(6) . ? N4A C15A 1.510(12) . ? C1A C2A 1.382(7) . ? C2A C3A 1.378(7) . ? C3A C4A 1.391(7) . ? C4A C5A 1.396(8) . ? C6A C7A 1.515(7) . ? C6A C9A 1.516(7) . ? C6A C8A 1.523(7) . ? C10A C11A 1.376(7) . ? C11A C12A 1.374(7) . ? C12A C13A 1.384(7) . ? C14A C13A 1.401(7) . ? C15A C16A 1.499(7) . ? C15A C18A 1.501(7) . ? C15A C17A 1.503(7) . ? N1B C4B 1.368(8) . ? N1B C1B 1.371(8) . ? N2B C5B 1.289(9) . ? N2B C6B 1.59(3) . ? N3B C13B 1.370(8) . ? N3B C10B 1.371(8) . ? N4B C14B 1.285(9) . ? N4B C15B 1.48(3) . ? C1B C2B 1.383(9) . ? C2B C3B 1.384(9) . ? C3B C4B 1.385(9) . ? C4B C5B 1.398(10) . ? C6B C9B 1.519(8) . ? C6B C7B 1.520(8) . ? C6B C8B 1.522(8) . ? C10B C11B 1.376(9) . ? C11B C12B 1.375(9) . ? C12B C13B 1.374(9) . ? C13B C14B 1.391(10) . ? C15B C17B 1.499(9) . ? C15B C16B 1.501(9) . ? C15B C18B 1.502(9) . ? 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 N5 Dy1 N3B 132.3(16) . . ? N5 Dy1 N1B 134.0(11) . . ? N3B Dy1 N1B 93.7(19) . . ? N5 Dy1 N1A 129.3(5) . . ? N3B Dy1 N1A 8.3(8) . . ? N1B Dy1 N1A 96.0(11) . . ? N5 Dy1 N3A 128.3(4) . . ? N3B Dy1 N3A 99.1(16) . . ? N1B Dy1 N3A 9.0(9) . . ? N1A Dy1 N3A 102.3(7) . . ? N5 Dy1 N4B 103.6(3) . . ? N3B Dy1 N4B 72.2(5) . . ? N1B Dy1 N4B 87.7(6) . . ? N1A Dy1 N4B 64.5(3) . . ? N3A Dy1 N4B 96.2(4) . . ? N5 Dy1 N2A 104.92(15) . . ? N3B Dy1 N2A 63.8(4) . . ? N1B Dy1 N2A 95.8(8) . . ? N1A Dy1 N2A 71.6(2) . . ? N3A Dy1 N2A 91.7(3) . . ? N4B Dy1 N2A 136.1(3) . . ? N5 Dy1 N4A 105.37(14) . . ? N3B Dy1 N4A 93.4(7) . . ? N1B Dy1 N4A 64.2(6) . . ? N1A Dy1 N4A 87.3(3) . . ? N3A Dy1 N4A 71.3(2) . . ? N4B Dy1 N4A 30.4(3) . . ? N2A Dy1 N4A 149.62(16) . . ? N5 Dy1 N2B 105.7(3) . . ? N3B Dy1 N2B 90.2(8) . . ? N1B Dy1 N2B 69.6(6) . . ? N1A Dy1 N2B 98.5(4) . . ? N3A Dy1 N2B 62.6(3) . . ? N4B Dy1 N2B 150.6(4) . . ? N2A Dy1 N2B 35.8(3) . . ? N4A Dy1 N2B 133.8(3) . . ? N5 Dy1 Si1 26.41(10) . . ? N3B Dy1 Si1 105.9(16) . . ? N1B Dy1 Si1 160.3(11) . . ? N1A Dy1 Si1 103.2(5) . . ? N3A Dy1 Si1 154.5(4) . . ? N4B Dy1 Si1 96.3(3) . . ? N2A Dy1 Si1 94.63(12) . . ? N4A Dy1 Si1 111.68(11) . . ? N2B Dy1 Si1 111.4(2) . . ? N5 Dy1 Si2 26.66(10) . . ? N3B Dy1 Si2 158.9(15) . . ? N1B Dy1 Si2 107.3(10) . . ? N1A Dy1 Si2 155.6(5) . . ? N3A Dy1 Si2 101.7(4) . . ? N4B Dy1 Si2 108.4(3) . . ? N2A Dy1 Si2 112.07(12) . . ? N4A Dy1 Si2 96.26(11) . . ? N2B Dy1 Si2 96.4(3) . . ? Si1 Dy1 Si2 53.07(4) . . ? N5 Si1 C19 108.0(2) . . ? N5 Si1 C21 116.1(3) . . ? C19 Si1 C21 103.1(4) . . ? N5 Si1 C20 115.8(3) . . ? C19 Si1 C20 107.1(4) . . ? C21 Si1 C20 105.7(4) . . ? N5 Si1 Dy1 35.61(12) . . ? C19 Si1 Dy1 72.36(19) . . ? C21 Si1 Dy1 125.2(3) . . ? C20 Si1 Dy1 128.3(3) . . ? N5 Si2 C24 113.9(3) . . ? N5 Si2 C22 107.7(2) . . ? C24 Si2 C22 107.4(4) . . ? N5 Si2 C23 114.3(4) . . ? C24 Si2 C23 106.8(5) . . ? C22 Si2 C23 106.3(4) . . ? N5 Si2 Dy1 35.48(12) . . ? C24 Si2 Dy1 124.6(3) . . ? C22 Si2 Dy1 72.29(19) . . ? C23 Si2 Dy1 127.0(3) . . ? Si1 N5 Si2 124.2(2) . . ? Si1 N5 Dy1 117.98(19) . . ? Si2 N5 Dy1 117.86(19) . . ? C1A N1A C4A 103.7(6) . . ? C1A N1A Dy1 142.6(6) . . ? C4A N1A Dy1 113.5(5) . . ? C5A N2A C6A 118.7(5) . . ? C5A N2A Dy1 111.7(4) . . ? C6A N2A Dy1 129.7(4) . . ? C10A N3A C13A 105.8(8) . . ? C10A N3A Dy1 138.6(6) . . ? C13A N3A Dy1 112.5(5) . . ? C14A N4A C15A 119.0(5) . . ? C14A N4A Dy1 111.2(4) . . ? C15A N4A Dy1 129.7(4) . . ? N1A C1A C2A 112.3(6) . . ? C3A C2A C1A 106.1(6) . . ? C2A C3A C4A 106.5(6) . . ? N1A C4A C3A 111.3(6) . . ? N1A C4A C5A 120.2(6) . . ? C3A C4A C5A 128.4(7) . . ? N2A C5A C4A 123.0(5) . . ? N2A C6A C7A 112.8(7) . . ? N2A C6A C9A 107.3(6) . . ? C7A C6A C9A 108.9(8) . . ? N2A C6A C8A 110.4(6) . . ? C7A C6A C8A 109.9(8) . . ? C9A C6A C8A 107.3(7) . . ? N3A C10A C11A 110.5(7) . . ? C12A C11A C10A 106.5(7) . . ? C11A C12A C13A 107.8(5) . . ? N4A C14A C13A 122.9(5) . . ? N3A C13A C12A 108.9(5) . . ? N3A C13A C14A 120.2(7) . . ? C12A C13A C14A 130.7(6) . . ? C16A C15A C18A 109.0(8) . . ? C16A C15A C17A 113.3(9) . . ? C18A C15A C17A 109.8(8) . . ? C16A C15A N4A 106.0(7) . . ? C18A C15A N4A 108.6(7) . . ? C17A C15A N4A 110.1(8) . . ? C4B N1B C1B 100.7(18) . . ? C4B N1B Dy1 115.2(15) . . ? C1B N1B Dy1 141(2) . . ? C5B N2B C6B 117.9(11) . . ? C5B N2B Dy1 113.9(9) . . ? C6B N2B Dy1 128.2(8) . . ? C13B N3B C10B 106.2(10) . . ? C13B N3B Dy1 112.6(9) . . ? C10B N3B Dy1 141.1(11) . . ? C14B N4B C15B 119.4(13) . . ? C14B N4B Dy1 111.8(9) . . ? C15B N4B Dy1 128.6(11) . . ? N1B C1B C2B 112.9(19) . . ? C1B C2B C3B 105.6(18) . . ? C2B C3B C4B 104.8(18) . . ? N1B C4B C3B 113(2) . . ? N1B C4B C5B 120(2) . . ? C3B C4B C5B 125(2) . . ? N2B C5B C4B 120.3(15) . . ? C9B C6B C7B 114(2) . . ? C9B C6B C8B 108.0(16) . . ? C7B C6B C8B 113.5(7) . . ? C9B C6B N2B 104.4(13) . . ? C7B C6B N2B 110.5(18) . . ? C8B C6B N2B 105.1(14) . . ? N3B C10B C11B 110.1(11) . . ? C12B C11B C10B 106.4(10) . . ? C13B C12B C11B 108.2(7) . . ? N3B C13B C12B 109.0(7) . . ? N3B C13B C14B 121.8(11) . . ? C12B C13B C14B 129.2(12) . . ? N4B C14B C13B 121.4(12) . . ? N4B C15B C17B 120(2) . . ? N4B C15B C16B 110.7(19) . . ? C17B C15B C16B 107(2) . . ? N4B C15B C18B 107.2(18) . . ? C17B C15B C18B 108(2) . . ? C16B C15B C18B 102(2) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.919 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.071 data_3c _database_code_depnum_ccdc_archive 'CCDC 896988' #TrackingRef 'CCDC 896988.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H44 N5 Si2 Yb' _chemical_formula_weight 631.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2342(9) _cell_length_b 9.3375(9) _cell_length_c 19.846(2) _cell_angle_alpha 86.9250(10) _cell_angle_beta 84.6240(10) _cell_angle_gamma 85.8500(10) _cell_volume 1697.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9954 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.61 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 642 _exptl_absorpt_coefficient_mu 2.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4036 _exptl_absorpt_correction_T_max 0.5736 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13050 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6589 _reflns_number_gt 6070 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Some highly disordered solvent peaks of solvent molecule were observed but could not be modelled satisfactorily. The SQUEEZE routine in PLATON was used to modify the HKL file. Restraints have been applied to refine the ligand which is affected by disorder. sadi 0.01 c10a c12a c10b c12b c10a c13a c10b c13b sadi 0.01 n3a c14a n3b c14b sadi 0.01 n1a c4a n1a c1a n1b c4b n1b c1b n3a c13a n3a c10a n3b c13b n3b c10b sadi 0.01 c1a c2a c2a c3a c3a c4a c1b c2b c2b c3b c3b c4b sadi 0.01 c10a c11a c10b c11b c11a c12a c11b c12b c12a c13a c12b c13b SADI 0.01 C13b C14b C13a C14a C4a C5a C4b C5b sadi 0.01 c6a c7a c6a c8a c6a c9a c6b c7b c6b c8b c6b c9b sadi 0.01 c15a c16a c15B c16b c15a c17a c15b c17b c15a c18a c15b c18b sadi 0.01 c5a n2a c5b n2b c14a n4a c14b n4b DELU 0.01 $C DELU 0.01 $N SIMU 0.01 $C SIMU 0.01 $N ; _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^)+(0.0339P)^2^+0.6929P] 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 6589 _refine_ls_number_parameters 497 _refine_ls_number_restraints 567 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.497 0.500 268 44 ' ' 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 N1B N 0.425(2) 0.030(2) 0.1190(10) 0.058(4) Uani 0.289(3) 1 d PGDU A 2 C1B C 0.4490(18) -0.0977(18) 0.0829(10) 0.066(3) Uani 0.289(3) 1 d PGDU A 2 H1B H 0.5261 -0.1666 0.0866 0.079 Uiso 0.289(3) 1 calc PR A 2 C2B C 0.335(2) -0.1020(15) 0.0400(9) 0.071(3) Uani 0.289(3) 1 d PGDU A 2 H2B H 0.3238 -0.1742 0.0107 0.085 Uiso 0.289(3) 1 calc PR A 2 C3B C 0.2399(17) 0.0233(17) 0.0497(10) 0.071(3) Uani 0.289(3) 1 d PGDU A 2 H3B H 0.1561 0.0476 0.0279 0.085 Uiso 0.289(3) 1 calc PR A 2 C4B C 0.296(2) 0.1051(17) 0.0985(12) 0.067(3) Uani 0.289(3) 1 d PGDU A 2 C19 C 0.3141(8) -0.0744(8) 0.2831(3) 0.133(3) Uani 1 1 d . . . H19A H 0.2484 -0.0063 0.2614 0.200 Uiso 1 1 calc R . . H19B H 0.2606 -0.1510 0.3050 0.200 Uiso 1 1 calc R . . H19C H 0.3866 -0.1129 0.2498 0.200 Uiso 1 1 calc R . . C20 C 0.5030(9) -0.1292(7) 0.3969(4) 0.146(3) Uani 1 1 d . . . H20A H 0.5942 -0.1573 0.3722 0.219 Uiso 1 1 calc R . . H20B H 0.4446 -0.2106 0.4041 0.219 Uiso 1 1 calc R . . H20C H 0.5209 -0.0947 0.4399 0.219 Uiso 1 1 calc R . . C21 C 0.2586(8) 0.0958(8) 0.4078(3) 0.139(3) Uani 1 1 d . . . H21A H 0.3011 0.1275 0.4463 0.209 Uiso 1 1 calc R . . H21B H 0.1910 0.0246 0.4226 0.209 Uiso 1 1 calc R . . H21C H 0.2081 0.1761 0.3859 0.209 Uiso 1 1 calc R . . C22 C 0.7223(9) 0.3630(9) 0.2837(3) 0.150(3) Uani 1 1 d . . . H22A H 0.7678 0.3055 0.2479 0.225 Uiso 1 1 calc R . . H22B H 0.7957 0.4070 0.3051 0.225 Uiso 1 1 calc R . . H22C H 0.6569 0.4364 0.2653 0.225 Uiso 1 1 calc R . . C23 C 0.7591(10) 0.1454(10) 0.3967(4) 0.171(4) Uani 1 1 d . . . H23A H 0.7283 0.0512 0.4101 0.257 Uiso 1 1 calc R . . H23B H 0.7718 0.1962 0.4363 0.257 Uiso 1 1 calc R . . H23C H 0.8498 0.1371 0.3688 0.257 Uiso 1 1 calc R . . C24 C 0.5072(10) 0.3688(8) 0.4072(3) 0.163(3) Uani 1 1 d . . . H24A H 0.4694 0.4517 0.3821 0.245 Uiso 1 1 calc R . . H24B H 0.5677 0.3984 0.4400 0.245 Uiso 1 1 calc R . . H24C H 0.4278 0.3191 0.4300 0.245 Uiso 1 1 calc R . . C1A C 0.8148(8) 0.2760(9) 0.0866(6) 0.0657(16) Uani 0.711(3) 1 d PDU A 1 H1A H 0.8857 0.2023 0.0939 0.079 Uiso 0.711(3) 1 calc PR A 1 C2A C 0.8341(8) 0.3924(8) 0.0404(4) 0.0696(16) Uani 0.711(3) 1 d PDU A 1 H2A H 0.9167 0.4090 0.0112 0.083 Uiso 0.711(3) 1 calc PR A 1 C3A C 0.7040(7) 0.4793(8) 0.0467(4) 0.0699(16) Uani 0.711(3) 1 d PDU A 1 H3A H 0.6830 0.5645 0.0221 0.084 Uiso 0.711(3) 1 calc PR A 1 C4A C 0.6114(7) 0.4136(7) 0.0973(4) 0.0604(14) Uani 0.711(3) 1 d PDU A 1 C5A C 0.4697(6) 0.4566(6) 0.1235(2) 0.0666(13) Uani 0.711(3) 1 d PDU A 1 H5A H 0.4260 0.5425 0.1069 0.080 Uiso 0.711(3) 1 calc PR A 1 C6A C 0.2527(13) 0.4404(11) 0.1987(4) 0.0833(18) Uani 0.711(3) 1 d PDU A 1 C7A C 0.1749(17) 0.5146(14) 0.1415(7) 0.130(4) Uani 0.711(3) 1 d PDU A 1 H7A1 H 0.1856 0.4547 0.1033 0.196 Uiso 0.711(3) 1 calc PR A 1 H7A2 H 0.2162 0.6046 0.1289 0.196 Uiso 0.711(3) 1 calc PR A 1 H7A3 H 0.0732 0.5316 0.1561 0.196 Uiso 0.711(3) 1 calc PR A 1 C8A C 0.2714(11) 0.5722(10) 0.2385(5) 0.121(3) Uani 0.711(3) 1 d PDU A 1 H8A1 H 0.1776 0.6106 0.2569 0.182 Uiso 0.711(3) 1 calc PR A 1 H8A2 H 0.3170 0.6438 0.2089 0.182 Uiso 0.711(3) 1 calc PR A 1 H8A3 H 0.3314 0.5452 0.2747 0.182 Uiso 0.711(3) 1 calc PR A 1 C9A C 0.1833(8) 0.3241(9) 0.2438(4) 0.102(2) Uani 0.711(3) 1 d PDU A 1 H9A1 H 0.2262 0.3160 0.2862 0.152 Uiso 0.711(3) 1 calc PR A 1 H9A2 H 0.1990 0.2342 0.2221 0.152 Uiso 0.711(3) 1 calc PR A 1 H9A3 H 0.0805 0.3482 0.2518 0.152 Uiso 0.711(3) 1 calc PR A 1 C10A C 0.2689(8) 0.0793(9) 0.0893(5) 0.0746(19) Uani 0.711(3) 1 d PDU A 1 H10A H 0.2016 0.1578 0.0948 0.089 Uiso 0.711(3) 1 calc PR A 1 C11A C 0.2583(8) -0.0273(8) 0.0457(4) 0.0760(17) Uani 0.711(3) 1 d PDU A 1 H11A H 0.1840 -0.0336 0.0177 0.091 Uiso 0.711(3) 1 calc PR A 1 C12A C 0.3750(7) -0.1216(7) 0.0508(4) 0.0687(16) Uani 0.711(3) 1 d PDU A 1 H12A H 0.3958 -0.2051 0.0272 0.082 Uiso 0.711(3) 1 calc PR A 1 C13A C 0.4571(7) -0.0708(7) 0.0973(3) 0.0580(14) Uani 0.711(3) 1 d PDU A 1 C14A C 0.5914(5) -0.1260(6) 0.1181(3) 0.0661(12) Uani 0.711(3) 1 d PDU A 1 H14A H 0.6335 -0.2113 0.1006 0.079 Uiso 0.711(3) 1 calc PR A 1 C15A C 0.8005(9) -0.1313(8) 0.1814(4) 0.0770(18) Uani 0.711(3) 1 d PDU A 1 C16A C 0.8588(8) -0.0310(8) 0.2280(4) 0.100(2) Uani 0.711(3) 1 d PDU A 1 H16A H 0.8582 0.0642 0.2071 0.151 Uiso 0.711(3) 1 calc PR A 1 H16B H 0.9567 -0.0638 0.2363 0.151 Uiso 0.711(3) 1 calc PR A 1 H16C H 0.7985 -0.0297 0.2701 0.151 Uiso 0.711(3) 1 calc PR A 1 C17A C 0.9081(13) -0.1564(16) 0.1190(7) 0.100(3) Uani 0.711(3) 1 d PDU A 1 H17A H 0.8775 -0.2328 0.0942 0.150 Uiso 0.711(3) 1 calc PR A 1 H17B H 1.0036 -0.1822 0.1331 0.150 Uiso 0.711(3) 1 calc PR A 1 H17C H 0.9106 -0.0701 0.0905 0.150 Uiso 0.711(3) 1 calc PR A 1 C18A C 0.7719(8) -0.2743(8) 0.2190(4) 0.102(2) Uani 0.711(3) 1 d PDU A 1 H18A H 0.6929 -0.2605 0.2536 0.154 Uiso 0.711(3) 1 calc PR A 1 H18B H 0.8580 -0.3115 0.2394 0.154 Uiso 0.711(3) 1 calc PR A 1 H18C H 0.7467 -0.3413 0.1876 0.154 Uiso 0.711(3) 1 calc PR A 1 C5B C 0.2479(13) 0.2328(13) 0.1280(6) 0.068(3) Uani 0.289(3) 1 d PDU A 2 H5B H 0.1622 0.2796 0.1145 0.081 Uiso 0.289(3) 1 calc PR A 2 C6B C 0.236(3) 0.428(4) 0.2021(11) 0.092(3) Uani 0.289(3) 1 d PDU A 2 C7B C 0.139(4) 0.460(3) 0.1445(16) 0.102(5) Uani 0.289(3) 1 d PDU A 2 H7B1 H 0.1601 0.5513 0.1224 0.152 Uiso 0.289(3) 1 calc PR A 2 H7B2 H 0.0388 0.4633 0.1624 0.152 Uiso 0.289(3) 1 calc PR A 2 H7B3 H 0.1573 0.3861 0.1125 0.152 Uiso 0.289(3) 1 calc PR A 2 C8B C 0.106(2) 0.380(3) 0.2480(12) 0.113(5) Uani 0.289(3) 1 d PDU A 2 H8B1 H 0.1022 0.2777 0.2467 0.169 Uiso 0.289(3) 1 calc PR A 2 H8B2 H 0.0180 0.4267 0.2328 0.169 Uiso 0.289(3) 1 calc PR A 2 H8B3 H 0.1154 0.4050 0.2936 0.169 Uiso 0.289(3) 1 calc PR A 2 C9B C 0.345(2) 0.486(2) 0.2454(10) 0.102(4) Uani 0.289(3) 1 d PDU A 2 H9B1 H 0.3623 0.4184 0.2824 0.153 Uiso 0.289(3) 1 calc PR A 2 H9B2 H 0.3056 0.5761 0.2629 0.153 Uiso 0.289(3) 1 calc PR A 2 H9B3 H 0.4347 0.5000 0.2183 0.153 Uiso 0.289(3) 1 calc PR A 2 C10B C 0.6386(17) 0.4485(17) 0.0856(11) 0.065(3) Uani 0.289(3) 1 d PDU A 2 H10B H 0.5539 0.5090 0.0871 0.078 Uiso 0.289(3) 1 calc PR A 2 C11B C 0.7601(18) 0.4693(19) 0.0432(11) 0.067(3) Uani 0.289(3) 1 d PDU A 2 H11B H 0.7763 0.5491 0.0141 0.080 Uiso 0.289(3) 1 calc PR A 2 C12B C 0.8534(17) 0.3523(19) 0.0512(11) 0.065(3) Uani 0.289(3) 1 d PDU A 2 H12B H 0.9458 0.3374 0.0286 0.077 Uiso 0.289(3) 1 calc PR A 2 C13B C 0.788(2) 0.261(2) 0.0978(14) 0.064(3) Uani 0.289(3) 1 d PDU A 2 C14B C 0.8422(11) 0.1248(11) 0.1184(6) 0.059(2) Uani 0.289(3) 1 d PDU A 2 H14B H 0.9347 0.0906 0.1012 0.071 Uiso 0.289(3) 1 calc PR A 2 C15B C 0.8334(19) -0.103(3) 0.1799(9) 0.080(3) Uani 0.289(3) 1 d PDU A 2 C16B C 0.7205(19) -0.176(2) 0.2276(10) 0.096(4) Uani 0.289(3) 1 d PDU A 2 H16D H 0.6504 -0.2144 0.2018 0.145 Uiso 0.289(3) 1 calc PR A 2 H16E H 0.6719 -0.1075 0.2578 0.145 Uiso 0.289(3) 1 calc PR A 2 H16F H 0.7676 -0.2529 0.2534 0.145 Uiso 0.289(3) 1 calc PR A 2 C17B C 0.875(4) -0.190(4) 0.1171(17) 0.088(5) Uani 0.289(3) 1 d PDU A 2 H17D H 0.9790 -0.2063 0.1108 0.132 Uiso 0.289(3) 1 calc PR A 2 H17E H 0.8407 -0.1370 0.0781 0.132 Uiso 0.289(3) 1 calc PR A 2 H17F H 0.8310 -0.2802 0.1228 0.132 Uiso 0.289(3) 1 calc PR A 2 C18B C 0.964(2) -0.087(2) 0.2195(11) 0.104(4) Uani 0.289(3) 1 d PDU A 2 H18D H 1.0006 -0.1799 0.2357 0.155 Uiso 0.289(3) 1 calc PR A 2 H18E H 0.9341 -0.0282 0.2573 0.155 Uiso 0.289(3) 1 calc PR A 2 H18F H 1.0383 -0.0422 0.1906 0.155 Uiso 0.289(3) 1 calc PR A 2 N5 N 0.5163(4) 0.1388(4) 0.30604(15) 0.0660(8) Uani 1 1 d . A . N1A N 0.6773(9) 0.2845(7) 0.1201(4) 0.0556(16) Uani 0.711(3) 1 d PDU A 1 N2A N 0.3982(5) 0.3821(5) 0.1697(2) 0.0608(10) Uani 0.711(3) 1 d PDU A 1 N3A N 0.3914(9) 0.0563(10) 0.1239(5) 0.0651(19) Uani 0.711(3) 1 d PDU A 1 N4A N 0.6587(4) -0.0622(5) 0.1609(2) 0.0602(10) Uani 0.711(3) 1 d PDU A 1 N2B N 0.3131(11) 0.2915(12) 0.1725(5) 0.061(2) Uani 0.289(3) 1 d PDU A 2 N3B N 0.658(2) 0.3242(16) 0.1266(10) 0.056(4) Uani 0.289(3) 1 d PDU A 2 N4B N 0.7664(10) 0.0455(10) 0.1607(5) 0.059(2) Uani 0.289(3) 1 d PDU A 2 Si1 Si 0.61764(19) 0.24626(18) 0.34781(7) 0.0949(4) Uani 1 1 d . A . Si2 Si 0.40458(16) 0.01658(16) 0.34731(6) 0.0846(3) Uani 1 1 d . A . Yb1 Yb 0.530044(14) 0.156886(14) 0.195256(6) 0.04949(6) Uani 1 1 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 N1B 0.060(8) 0.065(8) 0.051(6) -0.013(6) 0.002(6) -0.023(6) C1B 0.072(5) 0.066(5) 0.063(5) -0.014(5) -0.006(4) -0.012(4) C2B 0.072(6) 0.082(5) 0.063(5) -0.014(5) -0.014(5) -0.020(5) C3B 0.063(5) 0.088(6) 0.067(5) -0.012(5) -0.014(4) -0.013(5) C4B 0.054(6) 0.083(6) 0.068(6) -0.013(5) -0.010(5) -0.013(5) C19 0.175(7) 0.138(6) 0.093(4) 0.008(4) 0.003(4) -0.086(5) C20 0.184(7) 0.116(5) 0.128(5) 0.054(4) -0.007(5) 0.006(5) C21 0.143(6) 0.161(7) 0.105(4) -0.005(4) 0.039(4) -0.014(5) C22 0.203(8) 0.169(7) 0.097(4) -0.011(4) -0.027(4) -0.112(6) C23 0.179(8) 0.218(9) 0.132(6) -0.006(6) -0.102(6) -0.011(7) C24 0.244(10) 0.142(7) 0.110(5) -0.055(5) -0.005(6) -0.034(6) C1A 0.058(3) 0.069(3) 0.072(4) -0.002(3) -0.009(3) -0.017(3) C2A 0.072(3) 0.069(4) 0.069(3) 0.004(3) -0.002(3) -0.021(3) C3A 0.085(4) 0.061(3) 0.064(3) 0.007(2) -0.005(3) -0.013(3) C4A 0.076(3) 0.049(3) 0.056(3) 0.002(2) -0.007(2) -0.009(3) C5A 0.086(3) 0.052(3) 0.061(3) -0.002(2) -0.013(2) 0.007(2) C6A 0.078(4) 0.081(4) 0.086(4) -0.012(3) -0.003(3) 0.031(3) C7A 0.121(9) 0.124(9) 0.133(6) 0.019(6) -0.008(5) 0.061(6) C8A 0.129(6) 0.096(5) 0.135(6) -0.047(5) 0.012(5) 0.025(4) C9A 0.075(4) 0.114(5) 0.106(5) 0.002(4) 0.014(4) 0.026(4) C10A 0.063(3) 0.087(4) 0.076(4) -0.014(3) -0.010(3) -0.006(3) C11A 0.072(3) 0.091(4) 0.069(3) -0.014(3) -0.011(3) -0.018(3) C12A 0.074(4) 0.078(3) 0.060(3) -0.016(3) -0.010(3) -0.024(3) C13A 0.068(3) 0.056(3) 0.053(3) -0.014(2) 0.000(2) -0.017(2) C14A 0.068(3) 0.055(3) 0.073(3) -0.010(2) 0.007(2) -0.003(2) C15A 0.062(4) 0.069(4) 0.094(4) 0.011(3) -0.002(3) 0.019(3) C16A 0.073(4) 0.102(5) 0.128(5) 0.005(4) -0.038(4) 0.005(4) C17A 0.066(6) 0.099(8) 0.124(5) 0.012(5) 0.011(4) 0.026(5) C18A 0.088(4) 0.086(4) 0.124(5) 0.033(4) -0.001(4) 0.017(4) C5B 0.050(5) 0.086(6) 0.068(6) -0.008(5) -0.011(5) 0.003(5) C6B 0.083(6) 0.088(6) 0.099(6) -0.011(6) -0.003(5) 0.033(6) C7B 0.088(10) 0.089(11) 0.122(8) 0.007(8) -0.014(7) 0.033(9) C8B 0.097(9) 0.120(11) 0.113(9) -0.016(9) 0.018(8) 0.026(8) C9B 0.113(9) 0.080(8) 0.109(9) -0.013(8) -0.010(7) 0.019(7) C10B 0.074(5) 0.056(5) 0.062(5) 0.003(5) -0.001(4) -0.003(5) C11B 0.071(6) 0.065(5) 0.065(4) 0.003(4) -0.002(5) -0.013(5) C12B 0.064(5) 0.066(5) 0.064(5) 0.004(4) -0.002(4) -0.015(4) C13B 0.062(5) 0.066(5) 0.064(5) 0.001(4) -0.005(5) -0.017(5) C14B 0.047(5) 0.066(5) 0.066(5) -0.008(4) -0.006(4) -0.004(4) C15B 0.065(6) 0.074(7) 0.097(6) 0.006(5) -0.021(5) 0.023(5) C16B 0.084(7) 0.076(8) 0.123(9) 0.010(7) -0.005(7) 0.022(7) C17B 0.072(11) 0.074(10) 0.116(8) -0.012(7) -0.014(7) 0.017(8) C18B 0.086(8) 0.104(10) 0.124(10) -0.007(8) -0.047(8) 0.020(8) N5 0.0750(19) 0.0679(19) 0.0556(16) -0.0014(14) -0.0121(14) -0.0024(15) N1A 0.068(4) 0.043(4) 0.057(3) -0.009(3) -0.001(2) -0.013(3) N2A 0.064(2) 0.058(3) 0.058(2) -0.0070(19) -0.0053(19) 0.012(2) N3A 0.059(4) 0.066(4) 0.070(3) -0.016(2) 0.001(3) -0.005(3) N4A 0.053(2) 0.056(2) 0.069(2) -0.0019(19) -0.0022(18) 0.0030(18) N2B 0.057(5) 0.066(6) 0.058(5) 0.002(4) -0.006(4) 0.016(5) N3B 0.071(7) 0.039(8) 0.061(6) -0.025(6) 0.000(5) -0.010(6) N4B 0.055(5) 0.061(5) 0.059(5) -0.003(4) -0.006(4) 0.004(4) Si1 0.1207(11) 0.1073(11) 0.0634(7) -0.0079(7) -0.0259(7) -0.0276(9) Si2 0.1036(9) 0.0884(9) 0.0599(6) 0.0090(6) 0.0008(6) -0.0143(7) Yb1 0.05087(9) 0.04659(9) 0.05146(9) -0.00131(5) -0.00803(6) -0.00266(6) _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 N1B C1B 1.4200 . ? N1B C4B 1.4200 . ? N1B Yb1 2.294(11) . ? C1B C2B 1.4200 . ? C2B C3B 1.4200 . ? C3B C4B 1.4200 . ? C4B C5B 1.382(9) . ? C19 Si2 1.860(6) . ? C20 Si2 1.869(6) . ? C21 Si2 1.859(6) . ? C22 Si1 1.875(6) . ? C23 Si1 1.870(7) . ? C24 Si1 1.867(7) . ? C1A N1A 1.376(6) . ? C1A C2A 1.395(6) . ? C2A C3A 1.400(6) . ? C3A C4A 1.401(6) . ? C4A N1A 1.384(6) . ? C4A C5A 1.402(7) . ? C5A N2A 1.282(6) . ? C6A N2A 1.488(13) . ? C6A C7A 1.510(7) . ? C6A C9A 1.511(7) . ? C6A C8A 1.526(7) . ? C10A C11A 1.367(7) . ? C10A N3A 1.375(6) . ? C11A C12A 1.349(7) . ? C12A C13A 1.373(6) . ? C13A C14A 1.398(7) . ? C13A N3A 1.399(6) . ? C14A N4A 1.292(6) . ? C15A N4A 1.499(10) . ? C15A C16A 1.509(7) . ? C15A C18A 1.522(7) . ? C15A C17A 1.531(7) . ? C5B N2B 1.282(8) . ? C6B C7B 1.521(8) . ? C6B C8B 1.521(9) . ? C6B C9B 1.524(8) . ? C6B N2B 1.53(4) . ? C10B C11B 1.357(9) . ? C10B N3B 1.392(8) . ? C11B C12B 1.354(9) . ? C12B C13B 1.356(9) . ? C13B C14B 1.384(9) . ? C13B N3B 1.387(7) . ? C14B N4B 1.282(8) . ? C15B C16B 1.515(9) . ? C15B C18B 1.518(8) . ? C15B C17B 1.524(8) . ? C15B N4B 1.52(3) . ? N5 Si1 1.715(3) . ? N5 Si2 1.717(4) . ? N5 Yb1 2.188(3) . ? N1A Yb1 2.271(6) . ? N2A Yb1 2.407(4) . ? N3A Yb1 2.277(7) . ? N4A Yb1 2.389(4) . ? N2B Yb1 2.354(9) . ? N3B Yb1 2.332(16) . ? N4B Yb1 2.405(9) . ? Si1 Yb1 3.3681(13) . ? Si2 Yb1 3.3622(12) . ? 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 C1B N1B C4B 108.0 . . ? C1B N1B Yb1 140.8(10) . . ? C4B N1B Yb1 111.2(11) . . ? C2B C1B N1B 108.0 . . ? C3B C2B C1B 108.0 . . ? C4B C3B C2B 108.0 . . ? C5B C4B C3B 133.2(15) . . ? C5B C4B N1B 118.8(15) . . ? C3B C4B N1B 108.0 . . ? N1A C1A C2A 111.2(6) . . ? C1A C2A C3A 106.1(5) . . ? C2A C3A C4A 107.1(5) . . ? N1A C4A C3A 110.0(5) . . ? N1A C4A C5A 119.7(5) . . ? C3A C4A C5A 130.2(6) . . ? N2A C5A C4A 122.5(5) . . ? N2A C6A C7A 107.8(8) . . ? N2A C6A C9A 108.4(8) . . ? C7A C6A C9A 121.0(8) . . ? N2A C6A C8A 109.3(7) . . ? C7A C6A C8A 98.5(10) . . ? C9A C6A C8A 111.1(8) . . ? C11A C10A N3A 111.7(5) . . ? C12A C11A C10A 107.7(5) . . ? C11A C12A C13A 106.9(4) . . ? C12A C13A C14A 129.2(5) . . ? C12A C13A N3A 111.1(4) . . ? C14A C13A N3A 119.7(5) . . ? N4A C14A C13A 122.0(5) . . ? N4A C15A C16A 107.1(6) . . ? N4A C15A C18A 108.7(6) . . ? C16A C15A C18A 110.1(7) . . ? N4A C15A C17A 110.5(8) . . ? C16A C15A C17A 110.8(8) . . ? C18A C15A C17A 109.7(9) . . ? N2B C5B C4B 124.7(13) . . ? C7B C6B C8B 90.0(19) . . ? C7B C6B C9B 147(3) . . ? C8B C6B C9B 108.9(19) . . ? C7B C6B N2B 95.0(18) . . ? C8B C6B N2B 106(2) . . ? C9B C6B N2B 105(2) . . ? C11B C10B N3B 110.6(10) . . ? C12B C11B C10B 107.2(10) . . ? C11B C12B C13B 107.8(7) . . ? C12B C13B C14B 126.9(11) . . ? C12B C13B N3B 110.5(7) . . ? C14B C13B N3B 122.6(11) . . ? N4B C14B C13B 120.8(10) . . ? C16B C15B C18B 107.1(17) . . ? C16B C15B C17B 111(2) . . ? C18B C15B C17B 112(2) . . ? C16B C15B N4B 106.8(15) . . ? C18B C15B N4B 108.9(16) . . ? C17B C15B N4B 111(2) . . ? Si1 N5 Si2 122.89(18) . . ? Si1 N5 Yb1 118.78(17) . . ? Si2 N5 Yb1 118.33(17) . . ? C1A N1A C4A 105.5(5) . . ? C1A N1A Yb1 141.0(5) . . ? C4A N1A Yb1 113.5(4) . . ? C5A N2A C6A 119.2(5) . . ? C5A N2A Yb1 111.2(3) . . ? C6A N2A Yb1 129.6(4) . . ? C10A N3A C13A 102.6(5) . . ? C10A N3A Yb1 143.8(5) . . ? C13A N3A Yb1 113.1(4) . . ? C14A N4A C15A 118.2(5) . . ? C14A N4A Yb1 112.1(3) . . ? C15A N4A Yb1 129.7(4) . . ? C5B N2B C6B 116.3(11) . . ? C5B N2B Yb1 111.1(8) . . ? C6B N2B Yb1 132.5(9) . . ? C13B N3B C10B 102.7(9) . . ? C13B N3B Yb1 110.5(8) . . ? C10B N3B Yb1 142.2(14) . . ? C14B N4B C15B 117.4(10) . . ? C14B N4B Yb1 112.9(7) . . ? C15B N4B Yb1 129.7(8) . . ? N5 Si1 C24 114.2(3) . . ? N5 Si1 C23 114.1(3) . . ? C24 Si1 C23 107.3(4) . . ? N5 Si1 C22 108.7(2) . . ? C24 Si1 C22 106.9(4) . . ? C23 Si1 C22 105.0(4) . . ? N5 Si1 Yb1 34.72(11) . . ? C24 Si1 Yb1 126.5(3) . . ? C23 Si1 Yb1 124.5(3) . . ? C22 Si1 Yb1 74.00(18) . . ? N5 Si2 C19 108.6(2) . . ? N5 Si2 C21 114.5(3) . . ? C19 Si2 C21 107.4(3) . . ? N5 Si2 C20 114.0(3) . . ? C19 Si2 C20 106.2(4) . . ? C21 Si2 C20 105.7(3) . . ? N5 Si2 Yb1 34.95(10) . . ? C19 Si2 Yb1 73.67(17) . . ? C21 Si2 Yb1 127.5(2) . . ? C20 Si2 Yb1 124.8(2) . . ? N5 Yb1 N1A 130.5(3) . . ? N5 Yb1 N3A 128.7(3) . . ? N1A Yb1 N3A 100.8(4) . . ? N5 Yb1 N1B 130.9(7) . . ? N1A Yb1 N1B 98.1(7) . . ? N3A Yb1 N1B 9.7(5) . . ? N5 Yb1 N3B 125.8(6) . . ? N1A Yb1 N3B 10.4(4) . . ? N3A Yb1 N3B 104.4(8) . . ? N1B Yb1 N3B 103.3(9) . . ? N5 Yb1 N2B 103.4(2) . . ? N1A Yb1 N2B 95.5(3) . . ? N3A Yb1 N2B 64.7(3) . . ? N1B Yb1 N2B 74.1(5) . . ? N3B Yb1 N2B 88.3(6) . . ? N5 Yb1 N4A 104.21(13) . . ? N1A Yb1 N4A 90.38(18) . . ? N3A Yb1 N4A 73.0(2) . . ? N1B Yb1 N4A 63.5(5) . . ? N3B Yb1 N4A 100.7(3) . . ? N2B Yb1 N4A 137.7(3) . . ? N5 Yb1 N4B 104.1(2) . . ? N1A Yb1 N4B 63.0(3) . . ? N3A Yb1 N4B 100.5(3) . . ? N1B Yb1 N4B 90.9(5) . . ? N3B Yb1 N4B 72.2(4) . . ? N2B Yb1 N4B 152.2(3) . . ? N4A Yb1 N4B 35.6(3) . . ? N5 Yb1 N2A 104.43(13) . . ? N1A Yb1 N2A 72.84(19) . . ? N3A Yb1 N2A 87.1(2) . . ? N1B Yb1 N2A 95.2(5) . . ? N3B Yb1 N2A 63.8(4) . . ? N2B Yb1 N2A 28.9(3) . . ? N4A Yb1 N2A 151.24(15) . . ? N4B Yb1 N2A 135.8(2) . . ? N5 Yb1 Si2 26.71(9) . . ? N1A Yb1 Si2 156.9(3) . . ? N3A Yb1 Si2 102.2(3) . . ? N1B Yb1 Si2 104.2(6) . . ? N3B Yb1 Si2 152.3(6) . . ? N2B Yb1 Si2 96.4(3) . . ? N4A Yb1 Si2 94.06(10) . . ? N4B Yb1 Si2 110.1(2) . . ? N2A Yb1 Si2 110.62(10) . . ? N5 Yb1 Si1 26.50(9) . . ? N1A Yb1 Si1 104.2(3) . . ? N3A Yb1 Si1 154.6(3) . . ? N1B Yb1 Si1 157.3(6) . . ? N3B Yb1 Si1 99.3(6) . . ? N2B Yb1 Si1 107.7(2) . . ? N4A Yb1 Si1 111.41(11) . . ? N4B Yb1 Si1 95.2(2) . . ? N2A Yb1 Si1 95.54(10) . . ? Si2 Yb1 Si1 53.22(4) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.689 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.057 data_3d _database_code_depnum_ccdc_archive 'CCDC 896989' #TrackingRef 'CCDC 896989.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H44 Eu N5 Si2' _chemical_formula_weight 610.78 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2289(11) _cell_length_b 9.3704(11) _cell_length_c 20.064(2) _cell_angle_alpha 87.8760(10) _cell_angle_beta 84.7400(10) _cell_angle_gamma 86.2930(10) _cell_volume 1723.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6697 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.91 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 1.906 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7762 _exptl_absorpt_correction_T_max 0.8177 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14561 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.65 _reflns_number_total 7754 _reflns_number_gt 5707 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Some highly disordered solvent peaks of solvent molecule were observed but could not be modelled satisfactorily. The SQUEEZE routine in PLATON was used to modify the HKL file. Restraints have been applied to refine the ligand which is affected by disorder. SIMU 0.01 $N SIMU 0.01 $C DELU 0.01 $N DELU 0.01 $C sadi 0.01 c10a c12a c10b c12b c10a c13a c10b c13b sadi 0.01 n3a c14a n3b c14b sadi 0.01 n1a c4a n1a c1a n1b c4b n1b c1b n3a c13a n3a c10a n3b c13b n3b c10b sadi 0.01 c1a c2a c2a c3a c3a c4a c1b c2b c2b c3b c3b c4b sadi 0.01 c10a c11a c10b c11b c11a c12a c11b c12b c12a c13a c12b c13b sadi 0.01 C13b C14b C13a C14a C4a C5a C4b C5b sadi 0.01 c6a c7a c6a c8a c6a c9a c6b c7b c6B c8b c6b c9b sadi 0.01 c15a c16a c15b c16b c15a c17a c15b c17b c15a c18a c15b c18b sadi 0.01 C5a N2a C5b N2B C14a N4a C14b N4b ; _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^)+(0.0490P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7754 _refine_ls_number_parameters 496 _refine_ls_number_restraints 561 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.499 0.500 272 49 ' ' 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 C19 C 0.3108(8) -0.0599(7) 0.2847(3) 0.124(3) Uani 1 1 d . A . H19A H 0.2431 0.0084 0.2656 0.186 Uiso 1 1 calc R . . H19B H 0.2597 -0.1400 0.3037 0.186 Uiso 1 1 calc R . . H19C H 0.3837 -0.0923 0.2504 0.186 Uiso 1 1 calc R . . C20 C 0.2513(8) 0.1052(8) 0.4109(3) 0.128(3) Uani 1 1 d . A . H20A H 0.2890 0.1795 0.4349 0.193 Uiso 1 1 calc R . . H20B H 0.2163 0.0324 0.4421 0.193 Uiso 1 1 calc R . . H20C H 0.1727 0.1448 0.3865 0.193 Uiso 1 1 calc R . . C21 C 0.4969(9) -0.1231(7) 0.3974(4) 0.139(3) Uani 1 1 d . A . H21A H 0.4896 -0.2115 0.3756 0.208 Uiso 1 1 calc R . . H21B H 0.4534 -0.1304 0.4426 0.208 Uiso 1 1 calc R . . H21C H 0.5977 -0.1036 0.3976 0.208 Uiso 1 1 calc R . . C22 C 0.7143(9) 0.3694(8) 0.2876(3) 0.138(3) Uani 1 1 d . A . H22A H 0.7799 0.3094 0.2593 0.207 Uiso 1 1 calc R . . H22B H 0.7686 0.4360 0.3087 0.207 Uiso 1 1 calc R . . H22C H 0.6455 0.4208 0.2611 0.207 Uiso 1 1 calc R . . C23 C 0.5124(11) 0.3771(9) 0.4105(4) 0.170(4) Uani 1 1 d . A . H23A H 0.4697 0.4565 0.3860 0.255 Uiso 1 1 calc R . . H23B H 0.5762 0.4116 0.4406 0.255 Uiso 1 1 calc R . . H23C H 0.4368 0.3270 0.4356 0.255 Uiso 1 1 calc R . . C24 C 0.7564(10) 0.1599(11) 0.4016(4) 0.174(4) Uani 1 1 d . A . H24A H 0.8456 0.2080 0.3950 0.260 Uiso 1 1 calc R . . H24B H 0.7733 0.0636 0.3867 0.260 Uiso 1 1 calc R . . H24C H 0.7227 0.1583 0.4483 0.260 Uiso 1 1 calc R . . C1A C 0.2660(8) 0.0789(9) 0.0906(4) 0.0749(19) Uani 0.757(3) 1 d PDU A 1 H1A H 0.1967 0.1537 0.0999 0.090 Uiso 0.757(3) 1 calc PR A 1 C2A C 0.2545(8) -0.0272(8) 0.0436(4) 0.0722(16) Uani 0.757(3) 1 d PDU A 1 H2A H 0.1806 -0.0316 0.0154 0.087 Uiso 0.757(3) 1 calc PR A 1 C3A C 0.3755(8) -0.1251(8) 0.0474(4) 0.0713(17) Uani 0.757(3) 1 d PDU A 1 H3A H 0.3986 -0.2073 0.0231 0.086 Uiso 0.757(3) 1 calc PR A 1 C4A C 0.4543(10) -0.0697(11) 0.0969(6) 0.0648(16) Uani 0.757(3) 1 d PDU A 1 C5A C 0.5885(6) -0.1240(6) 0.1166(3) 0.0643(14) Uani 0.757(3) 1 d PDU A 1 H5A H 0.6309 -0.2072 0.0973 0.077 Uiso 0.757(3) 1 calc PR A 1 C6A C 0.7976(8) -0.1317(7) 0.1793(4) 0.0785(19) Uani 0.757(3) 1 d PDU A 1 C7A C 0.9094(10) -0.160(2) 0.1200(6) 0.104(3) Uani 0.757(3) 1 d PDU A 1 H7A H 0.8806 -0.2373 0.0951 0.155 Uiso 0.757(3) 1 calc PR A 1 H7B H 1.0030 -0.1850 0.1359 0.155 Uiso 0.757(3) 1 calc PR A 1 H7C H 0.9153 -0.0755 0.0916 0.155 Uiso 0.757(3) 1 calc PR A 1 C8A C 0.7679(9) -0.2703(7) 0.2184(4) 0.098(2) Uani 0.757(3) 1 d PDU A 1 H8A H 0.8503 -0.3000 0.2426 0.147 Uiso 0.757(3) 1 calc PR A 1 H8B H 0.7515 -0.3430 0.1880 0.147 Uiso 0.757(3) 1 calc PR A 1 H8C H 0.6831 -0.2553 0.2494 0.147 Uiso 0.757(3) 1 calc PR A 1 C9A C 0.8562(8) -0.0311(8) 0.2266(4) 0.100(2) Uani 0.757(3) 1 d PDU A 1 H9A H 0.9491 -0.0695 0.2391 0.151 Uiso 0.757(3) 1 calc PR A 1 H9B H 0.7893 -0.0210 0.2659 0.151 Uiso 0.757(3) 1 calc PR A 1 H9C H 0.8671 0.0608 0.2046 0.151 Uiso 0.757(3) 1 calc PR A 1 C10A C 0.8163(8) 0.2846(8) 0.0868(5) 0.0656(18) Uani 0.757(3) 1 d PDU A 1 H10A H 0.8877 0.2125 0.0941 0.079 Uiso 0.757(3) 1 calc PR A 1 C11A C 0.8320(9) 0.3958(8) 0.0397(4) 0.0710(18) Uani 0.757(3) 1 d PDU A 1 H11A H 0.9130 0.4111 0.0098 0.085 Uiso 0.757(3) 1 calc PR A 1 C12A C 0.7033(7) 0.4788(8) 0.0460(4) 0.0739(17) Uani 0.757(3) 1 d PDU A 1 H12A H 0.6811 0.5608 0.0205 0.089 Uiso 0.757(3) 1 calc PR A 1 C13A C 0.6122(7) 0.4185(7) 0.0972(4) 0.0636(17) Uani 0.757(3) 1 d PDU A 1 C14A C 0.4706(6) 0.4636(6) 0.1223(3) 0.0654(14) Uani 0.757(3) 1 d PDU A 1 H14A H 0.4273 0.5465 0.1039 0.078 Uiso 0.757(3) 1 calc PR A 1 C15A C 0.2488(10) 0.4549(8) 0.1967(4) 0.0833(19) Uani 0.757(3) 1 d PDU A 1 C16A C 0.1824(9) 0.3362(9) 0.2415(4) 0.103(2) Uani 0.757(3) 1 d PDU A 1 H16A H 0.0837 0.3653 0.2567 0.154 Uiso 0.757(3) 1 calc PR A 1 H16B H 0.2382 0.3181 0.2794 0.154 Uiso 0.757(3) 1 calc PR A 1 H16C H 0.1838 0.2505 0.2166 0.154 Uiso 0.757(3) 1 calc PR A 1 C17A C 0.1528(10) 0.4911(10) 0.1394(5) 0.109(3) Uani 0.757(3) 1 d PDU A 1 H17A H 0.0549 0.5158 0.1576 0.163 Uiso 0.757(3) 1 calc PR A 1 H17B H 0.1534 0.4097 0.1117 0.163 Uiso 0.757(3) 1 calc PR A 1 H17C H 0.1900 0.5706 0.1131 0.163 Uiso 0.757(3) 1 calc PR A 1 C18A C 0.2659(11) 0.5901(9) 0.2345(5) 0.123(3) Uani 0.757(3) 1 d PDU A 1 H18A H 0.1721 0.6263 0.2535 0.185 Uiso 0.757(3) 1 calc PR A 1 H18B H 0.3079 0.6610 0.2041 0.185 Uiso 0.757(3) 1 calc PR A 1 H18C H 0.3286 0.5681 0.2696 0.185 Uiso 0.757(3) 1 calc PR A 1 C1B C 0.640(3) 0.450(3) 0.0870(17) 0.067(3) Uani 0.243(3) 1 d PDU A 2 H1B H 0.5531 0.5058 0.0867 0.080 Uiso 0.243(3) 1 calc PR A 2 C2B C 0.764(2) 0.475(3) 0.0430(14) 0.067(3) Uani 0.243(3) 1 d PDU A 2 H2B H 0.7796 0.5539 0.0141 0.080 Uiso 0.243(3) 1 calc PR A 2 C3B C 0.860(3) 0.355(3) 0.0531(14) 0.066(3) Uani 0.243(3) 1 d PDU A 2 H3B H 0.9522 0.3356 0.0316 0.079 Uiso 0.243(3) 1 calc PR A 2 C4B C 0.785(3) 0.269(2) 0.1026(17) 0.063(3) Uani 0.243(3) 1 d PDU A 2 C5B C 0.8439(18) 0.1313(17) 0.1171(8) 0.063(3) Uani 0.243(3) 1 d PDU A 2 H5B H 0.9344 0.0992 0.0971 0.075 Uiso 0.243(3) 1 calc PR A 2 C6B C 0.8317(18) -0.097(3) 0.1813(10) 0.083(4) Uani 0.243(3) 1 d PDU A 2 C7B C 0.8733(19) -0.168(6) 0.1149(17) 0.080(5) Uani 0.243(3) 1 d PDU A 2 H7D H 0.8913 -0.2695 0.1226 0.119 Uiso 0.243(3) 1 calc PR A 2 H7E H 0.9598 -0.1290 0.0935 0.119 Uiso 0.243(3) 1 calc PR A 2 H7F H 0.7951 -0.1519 0.0866 0.119 Uiso 0.243(3) 1 calc PR A 2 C8B C 0.9666(19) -0.077(3) 0.2173(11) 0.092(5) Uani 0.243(3) 1 d PRDU A 2 H8D H 0.9932 -0.1658 0.2358 0.137 Uiso 0.243(3) 1 d PR A 2 H8E H 0.9445 -0.0164 0.2543 0.137 Uiso 0.243(3) 1 d PR A 2 H8F H 1.0385 -0.0270 0.1921 0.137 Uiso 0.243(3) 1 d PR A 2 C9B C 0.709(2) -0.156(2) 0.2283(13) 0.092(5) Uani 0.243(3) 1 d PDU A 2 H9D H 0.7090 -0.2575 0.2235 0.139 Uiso 0.243(3) 1 calc PR A 2 H9E H 0.6176 -0.1114 0.2172 0.139 Uiso 0.243(3) 1 calc PR A 2 H9F H 0.7242 -0.1362 0.2736 0.139 Uiso 0.243(3) 1 calc PR A 2 C10B C 0.439(3) -0.080(3) 0.0845(18) 0.065(3) Uani 0.243(3) 1 d PDU A 2 H10B H 0.5252 -0.1375 0.0833 0.078 Uiso 0.243(3) 1 calc PR A 2 C11B C 0.328(3) -0.089(2) 0.0430(14) 0.069(3) Uani 0.243(3) 1 d PDU A 2 H11B H 0.3165 -0.1612 0.0139 0.083 Uiso 0.243(3) 1 calc PR A 2 C12B C 0.238(2) 0.033(2) 0.0543(13) 0.073(3) Uani 0.243(3) 1 d PDU A 2 H12B H 0.1501 0.0550 0.0357 0.088 Uiso 0.243(3) 1 calc PR A 2 C13B C 0.300(3) 0.118(2) 0.0978(12) 0.075(3) Uani 0.243(3) 1 d PDU A 2 C14B C 0.2340(19) 0.2409(19) 0.1262(9) 0.074(3) Uani 0.243(3) 1 d PDU A 2 H14B H 0.1458 0.2826 0.1139 0.089 Uiso 0.243(3) 1 calc PR A 2 C15B C 0.237(3) 0.427(3) 0.2011(12) 0.092(4) Uani 0.243(3) 1 d PDU A 2 C16B C 0.324(3) 0.490(2) 0.2528(13) 0.096(4) Uani 0.243(3) 1 d PDU A 2 H16D H 0.2672 0.5666 0.2747 0.144 Uiso 0.243(3) 1 calc PR A 2 H16E H 0.4122 0.5251 0.2308 0.144 Uiso 0.243(3) 1 calc PR A 2 H16F H 0.3484 0.4164 0.2854 0.144 Uiso 0.243(3) 1 calc PR A 2 C17B C 0.207(3) 0.560(3) 0.1568(16) 0.106(5) Uani 0.243(3) 1 d PDU A 2 H17D H 0.2560 0.5464 0.1129 0.159 Uiso 0.243(3) 1 calc PR A 2 H17E H 0.2420 0.6419 0.1760 0.159 Uiso 0.243(3) 1 calc PR A 2 H17F H 0.1039 0.5748 0.1534 0.159 Uiso 0.243(3) 1 calc PR A 2 C18B C 0.103(3) 0.414(3) 0.2514(15) 0.109(5) Uani 0.243(3) 1 d PDU A 2 H18D H 0.1306 0.3599 0.2902 0.163 Uiso 0.243(3) 1 calc PR A 2 H18E H 0.0300 0.3664 0.2312 0.163 Uiso 0.243(3) 1 calc PR A 2 H18F H 0.0649 0.5078 0.2642 0.163 Uiso 0.243(3) 1 calc PR A 2 Eu1 Eu 0.52728(2) 0.16289(2) 0.198836(10) 0.05059(9) Uani 1 1 d . A . N5 N 0.5126(4) 0.1459(4) 0.31230(17) 0.0628(9) Uani 1 1 d . A . N1A N 0.3928(17) 0.0565(13) 0.1206(6) 0.065(2) Uani 0.757(3) 1 d PDU A 1 N2A N 0.6569(5) -0.0638(5) 0.1605(2) 0.0570(11) Uani 0.757(3) 1 d PDU A 1 N3A N 0.6818(8) 0.2957(8) 0.1211(4) 0.0510(17) Uani 0.757(3) 1 d PDU A 1 N4A N 0.3973(5) 0.3951(5) 0.1700(2) 0.0614(12) Uani 0.757(3) 1 d PDU A 1 N1B N 0.658(4) 0.335(3) 0.1301(15) 0.056(5) Uani 0.243(3) 1 d PDU A 2 N2B N 0.7697(15) 0.0493(15) 0.1588(7) 0.059(3) Uani 0.243(3) 1 d PDU A 2 N3B N 0.399(6) 0.028(4) 0.1274(19) 0.063(5) Uani 0.243(3) 1 d PDU A 2 N4B N 0.3052(16) 0.2934(16) 0.1711(7) 0.066(3) Uani 0.243(3) 1 d PDU A 2 Si1 Si 0.39952(18) 0.02542(17) 0.35120(7) 0.0821(4) Uani 1 1 d . . . Si2 Si 0.6153(2) 0.25688(19) 0.35262(8) 0.0906(5) Uani 1 1 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 C19 0.154(6) 0.130(6) 0.093(5) 0.002(4) 0.003(4) -0.074(5) C20 0.127(6) 0.144(6) 0.106(5) -0.018(4) 0.044(4) -0.018(5) C21 0.178(8) 0.101(5) 0.131(6) 0.043(4) -0.003(5) -0.003(5) C22 0.185(8) 0.136(6) 0.106(5) -0.010(4) -0.026(5) -0.092(6) C23 0.243(11) 0.136(7) 0.135(7) -0.079(6) 0.005(7) -0.026(7) C24 0.169(8) 0.217(10) 0.155(8) 0.020(7) -0.105(7) -0.054(7) C1A 0.065(4) 0.095(4) 0.065(4) -0.016(3) -0.007(3) -0.008(3) C2A 0.073(3) 0.088(4) 0.060(3) -0.013(3) -0.011(3) -0.017(3) C3A 0.082(4) 0.071(4) 0.064(3) -0.013(3) -0.004(3) -0.019(3) C4A 0.069(3) 0.065(3) 0.062(4) -0.007(3) -0.002(3) -0.017(3) C5A 0.069(3) 0.056(3) 0.066(3) -0.004(3) 0.003(3) -0.006(3) C6A 0.064(4) 0.071(4) 0.097(4) 0.008(3) -0.007(3) 0.015(3) C7A 0.077(5) 0.101(6) 0.125(6) 0.010(5) 0.012(5) 0.020(6) C8A 0.106(6) 0.072(4) 0.110(6) 0.017(4) -0.001(4) 0.020(4) C9A 0.068(4) 0.105(5) 0.131(6) 0.006(4) -0.037(4) 0.008(4) C10A 0.056(4) 0.075(4) 0.066(5) -0.002(3) 0.000(3) -0.017(3) C11A 0.078(4) 0.073(4) 0.063(4) 0.000(3) 0.000(3) -0.027(3) C12A 0.088(4) 0.067(3) 0.067(3) 0.003(3) 0.000(4) -0.021(3) C13A 0.077(4) 0.057(4) 0.058(4) 0.002(3) -0.005(3) -0.012(3) C14A 0.084(4) 0.046(3) 0.065(3) 0.002(3) -0.007(3) 0.002(3) C15A 0.075(4) 0.078(4) 0.092(4) -0.005(3) -0.002(3) 0.028(3) C16A 0.092(5) 0.106(5) 0.101(5) -0.005(4) 0.018(4) 0.022(4) C17A 0.089(6) 0.113(6) 0.119(6) -0.002(5) -0.020(4) 0.038(5) C18A 0.134(7) 0.096(5) 0.135(7) -0.045(5) 0.004(6) 0.023(5) C1B 0.078(5) 0.058(5) 0.063(5) 0.002(5) 0.002(5) -0.013(5) C2B 0.075(6) 0.063(5) 0.062(5) 0.006(5) 0.004(5) -0.021(5) C3B 0.068(5) 0.068(5) 0.064(6) 0.004(5) 0.001(5) -0.021(5) C4B 0.062(7) 0.067(6) 0.059(7) 0.008(5) -0.003(6) -0.020(6) C5B 0.055(6) 0.073(6) 0.061(7) 0.001(6) -0.005(6) -0.012(6) C6B 0.064(6) 0.079(7) 0.103(6) 0.004(6) -0.017(6) 0.021(6) C7B 0.053(9) 0.078(10) 0.107(8) -0.004(8) -0.021(7) 0.018(9) C8B 0.076(9) 0.084(11) 0.117(11) -0.020(10) -0.028(9) 0.021(9) C9B 0.089(9) 0.061(9) 0.122(10) 0.014(9) 0.000(8) 0.012(8) C10B 0.069(5) 0.067(5) 0.061(6) -0.007(5) -0.004(5) -0.016(5) C11B 0.072(5) 0.077(5) 0.061(5) -0.011(4) -0.007(5) -0.015(4) C12B 0.070(5) 0.088(6) 0.064(5) -0.014(5) -0.008(5) -0.013(5) C13B 0.069(7) 0.093(7) 0.065(6) -0.019(5) -0.009(6) -0.015(6) C14B 0.064(7) 0.094(7) 0.066(7) -0.014(6) -0.007(6) -0.007(6) C15B 0.079(7) 0.091(7) 0.101(7) -0.006(6) -0.002(6) 0.031(6) C16B 0.103(9) 0.063(9) 0.118(10) -0.019(8) -0.013(8) 0.041(8) C17B 0.095(11) 0.099(10) 0.119(10) -0.001(8) -0.009(8) 0.026(9) C18B 0.098(10) 0.101(12) 0.118(12) -0.019(10) 0.024(9) 0.028(9) Eu1 0.05226(13) 0.04730(12) 0.05255(13) -0.00313(8) -0.00507(8) -0.00437(8) N5 0.076(2) 0.061(2) 0.053(2) -0.0027(17) -0.0083(17) -0.0052(18) N1A 0.074(4) 0.062(6) 0.062(4) -0.002(4) -0.013(3) -0.013(4) N2A 0.063(3) 0.045(2) 0.063(3) -0.002(2) -0.001(2) -0.003(2) N3A 0.053(4) 0.048(5) 0.051(3) -0.012(3) 0.004(3) -0.006(3) N4A 0.073(3) 0.046(3) 0.062(3) -0.008(2) -0.001(2) 0.014(2) N1B 0.065(8) 0.041(10) 0.061(8) -0.024(8) 0.006(7) 0.004(7) N2B 0.056(6) 0.060(7) 0.061(7) 0.003(6) -0.008(6) -0.002(6) N3B 0.077(8) 0.056(10) 0.061(8) -0.007(9) -0.008(7) -0.025(7) N4B 0.066(7) 0.068(7) 0.059(7) 0.004(6) 0.008(6) 0.012(6) Si1 0.1028(11) 0.0807(9) 0.0611(8) 0.0046(7) 0.0059(8) -0.0149(8) Si2 0.1192(13) 0.0938(11) 0.0639(9) -0.0117(8) -0.0191(9) -0.0260(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C19 Si1 1.859(6) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 Si1 1.871(6) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 Si1 1.870(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 Si2 1.858(7) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 Si2 1.810(7) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 Si2 1.872(8) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C1A N1A 1.365(8) . ? C1A C2A 1.411(7) . ? C1A H1A 0.9300 . ? C2A C3A 1.404(7) . ? C2A H2A 0.9300 . ? C3A C4A 1.415(7) . ? C3A H3A 0.9300 . ? C4A N1A 1.360(6) . ? C4A C5A 1.394(8) . ? C4A Eu1 3.187(7) . ? C5A N2A 1.296(6) . ? C5A Eu1 3.199(6) . ? C5A H5A 0.9300 . ? C6A N2A 1.482(9) . ? C6A C9A 1.519(7) . ? C6A C8A 1.520(6) . ? C6A C7A 1.521(7) . ? C7A H7A 0.9600 . ? C7A H7B 0.9600 . ? C7A H7C 0.9600 . ? C8A H8A 0.9600 . ? C8A H8B 0.9600 . ? C8A H8C 0.9600 . ? C9A H9A 0.9600 . ? C9A H9B 0.9600 . ? C9A H9C 0.9600 . ? C9A H8E 1.0472 . ? C10A N3A 1.362(6) . ? C10A C11A 1.386(7) . ? C10A H10A 0.9300 . ? C11A C12A 1.375(7) . ? C11A H11A 0.9300 . ? C12A C13A 1.393(7) . ? C12A H12A 0.9300 . ? C13A N3A 1.374(6) . ? C13A C14A 1.402(7) . ? C13A Eu1 3.178(6) . ? C14A N4A 1.295(6) . ? C14A Eu1 3.195(5) . ? C14A H14A 0.9300 . ? C15A N4A 1.506(11) . ? C15A C18A 1.524(7) . ? C15A C16A 1.528(7) . ? C15A C17A 1.529(7) . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C17A H17A 0.9600 . ? C17A H17B 0.9600 . ? C17A H17C 0.9600 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C1B N1B 1.366(8) . ? C1B C2B 1.409(10) . ? C1B H1B 0.9300 . ? C2B C3B 1.408(10) . ? C2B H2B 0.9300 . ? C3B C4B 1.411(10) . ? C3B H3B 0.9300 . ? C4B N1B 1.368(8) . ? C4B C5B 1.398(10) . ? C4B Eu1 3.12(3) . ? C5B N2B 1.294(9) . ? C5B Eu1 3.219(16) . ? C5B H5B 0.9300 . ? C6B N2B 1.52(3) . ? C6B C7B 1.520(8) . ? C6B C9B 1.521(8) . ? C6B C8B 1.521(8) . ? C7B H7D 0.9600 . ? C7B H7E 0.9600 . ? C7B H7F 0.9600 . ? C8B H8D 0.9301 . ? C8B H8E 0.9490 . ? C8B H8F 0.9338 . ? C9B H9D 0.9600 . ? C9B H9E 0.9600 . ? C9B H9F 0.9600 . ? C10B N3B 1.365(8) . ? C10B C11B 1.387(9) . ? C10B H10B 0.9300 . ? C11B C12B 1.382(9) . ? C11B H11B 0.9300 . ? C12B C13B 1.383(9) . ? C12B H12B 0.9300 . ? C13B N3B 1.365(8) . ? C13B C14B 1.387(10) . ? C13B Eu1 3.11(2) . ? C14B N4B 1.292(9) . ? C14B Eu1 3.221(17) . ? C14B H14B 0.9300 . ? C15B N4B 1.49(3) . ? C15B C17B 1.525(9) . ? C15B C16B 1.526(9) . ? C15B C18B 1.528(9) . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C17B H17D 0.9600 . ? C17B H17E 0.9600 . ? C17B H17F 0.9600 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? Eu1 N5 2.268(4) . ? Eu1 N1A 2.374(10) . ? Eu1 N3B 2.38(3) . ? Eu1 N3A 2.387(7) . ? Eu1 N1B 2.40(3) . ? Eu1 N4B 2.417(15) . ? Eu1 N2A 2.482(4) . ? Eu1 N4A 2.491(4) . ? Eu1 N2B 2.491(14) . ? N5 Si1 1.706(4) . ? N5 Si2 1.722(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si1 C21 H21A 109.5 . . ? Si1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si2 C24 H24A 109.5 . . ? Si2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1A C1A C2A 110.6(6) . . ? N1A C1A H1A 124.7 . . ? C2A C1A H1A 124.7 . . ? C3A C2A C1A 107.3(6) . . ? C3A C2A H2A 126.4 . . ? C1A C2A H2A 126.4 . . ? C2A C3A C4A 104.0(6) . . ? C2A C3A H3A 128.0 . . ? C4A C3A H3A 128.0 . . ? N1A C4A C5A 120.5(7) . . ? N1A C4A C3A 112.7(6) . . ? C5A C4A C3A 126.5(7) . . ? N1A C4A Eu1 42.7(5) . . ? C5A C4A Eu1 77.9(4) . . ? C3A C4A Eu1 155.2(5) . . ? N2A C5A C4A 122.9(6) . . ? N2A C5A Eu1 46.0(3) . . ? C4A C5A Eu1 76.9(4) . . ? N2A C5A H5A 118.6 . . ? C4A C5A H5A 118.6 . . ? Eu1 C5A H5A 164.4 . . ? N2A C6A C9A 106.5(6) . . ? N2A C6A C8A 108.5(6) . . ? C9A C6A C8A 107.5(7) . . ? N2A C6A C7A 114.0(7) . . ? C9A C6A C7A 109.9(8) . . ? C8A C6A C7A 110.3(10) . . ? N3A C10A C11A 110.6(7) . . ? N3A C10A H10A 124.7 . . ? C11A C10A H10A 124.7 . . ? C12A C11A C10A 106.1(7) . . ? C12A C11A H11A 127.0 . . ? C10A C11A H11A 127.0 . . ? C11A C12A C13A 108.1(5) . . ? C11A C12A H12A 125.9 . . ? C13A C12A H12A 125.9 . . ? N3A C13A C12A 108.6(5) . . ? N3A C13A C14A 121.7(6) . . ? C12A C13A C14A 129.7(6) . . ? N3A C13A Eu1 43.9(3) . . ? C12A C13A Eu1 151.7(4) . . ? C14A C13A Eu1 78.0(3) . . ? N4A C14A C13A 123.0(5) . . ? N4A C14A Eu1 46.6(3) . . ? C13A C14A Eu1 76.6(3) . . ? N4A C14A H14A 118.5 . . ? C13A C14A H14A 118.5 . . ? Eu1 C14A H14A 164.0 . . ? N4A C15A C18A 109.0(6) . . ? N4A C15A C16A 105.8(6) . . ? C18A C15A C16A 112.8(7) . . ? N4A C15A C17A 110.6(6) . . ? C18A C15A C17A 109.4(7) . . ? C16A C15A C17A 109.2(8) . . ? N1B C1B C2B 114(2) . . ? N1B C1B H1B 123.0 . . ? C2B C1B H1B 123.0 . . ? C3B C2B C1B 104(2) . . ? C3B C2B H2B 128.0 . . ? C1B C2B H2B 128.0 . . ? C2B C3B C4B 105(2) . . ? C2B C3B H3B 127.3 . . ? C4B C3B H3B 127.3 . . ? N1B C4B C5B 128(2) . . ? N1B C4B C3B 113(2) . . ? C5B C4B C3B 119(2) . . ? N1B C4B Eu1 46.9(13) . . ? C5B C4B Eu1 81.4(13) . . ? C3B C4B Eu1 158.4(17) . . ? N2B C5B C4B 118.7(18) . . ? N2B C5B Eu1 45.6(9) . . ? C4B C5B Eu1 73.2(13) . . ? N2B C5B H5B 120.6 . . ? C4B C5B H5B 120.6 . . ? Eu1 C5B H5B 166.1 . . ? N2B C6B C7B 102(3) . . ? N2B C6B C9B 104.0(15) . . ? C7B C6B C9B 119(3) . . ? N2B C6B C8B 108.3(19) . . ? C7B C6B C8B 110.7(7) . . ? C9B C6B C8B 112.0(18) . . ? C6B C7B H7D 109.5 . . ? C6B C7B H7E 109.5 . . ? H7D C7B H7E 109.5 . . ? C6B C7B H7F 109.5 . . ? H7D C7B H7F 109.5 . . ? H7E C7B H7F 109.5 . . ? C6B C8B H8D 105.9 . . ? C6B C8B H8E 111.3 . . ? H8D C8B H8E 105.2 . . ? C6B C8B H8F 114.7 . . ? H8D C8B H8F 118.0 . . ? H8E C8B H8F 101.4 . . ? C6B C9B H9D 109.5 . . ? C6B C9B H9E 109.5 . . ? H9D C9B H9E 109.5 . . ? C6B C9B H9F 109.5 . . ? H9D C9B H9F 109.5 . . ? H9E C9B H9F 109.5 . . ? N3B C10B C11B 107.8(16) . . ? N3B C10B H10B 126.1 . . ? C11B C10B H10B 126.1 . . ? C12B C11B C10B 105.3(10) . . ? C12B C11B H11B 127.4 . . ? C10B C11B H11B 127.4 . . ? C11B C12B C13B 108.7(7) . . ? C11B C12B H12B 125.6 . . ? C13B C12B H12B 125.6 . . ? N3B C13B C12B 105.3(15) . . ? N3B C13B C14B 124.0(13) . . ? C12B C13B C14B 125.4(16) . . ? N3B C13B Eu1 46.3(15) . . ? C12B C13B Eu1 151.4(10) . . ? C14B C13B Eu1 81.9(9) . . ? N4B C14B C13B 114.6(14) . . ? N4B C14B Eu1 41.8(9) . . ? C13B C14B Eu1 72.9(9) . . ? N4B C14B H14B 122.7 . . ? C13B C14B H14B 122.7 . . ? Eu1 C14B H14B 164.4 . . ? N4B C15B C17B 120(2) . . ? N4B C15B C16B 114(2) . . ? C17B C15B C16B 101(2) . . ? N4B C15B C18B 118(2) . . ? C17B C15B C18B 107(3) . . ? C16B C15B C18B 92(2) . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C15B C17B H17D 109.5 . . ? C15B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C15B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C15B C18B H18D 109.5 . . ? C15B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C15B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? N5 Eu1 N1A 131.1(5) . . ? N5 Eu1 N3B 126.4(15) . . ? N1A Eu1 N3B 7.2(11) . . ? N5 Eu1 N3A 130.8(3) . . ? N1A Eu1 N3A 98.1(6) . . ? N3B Eu1 N3A 102.6(15) . . ? N5 Eu1 N1B 125.7(9) . . ? N1A Eu1 N1B 102.3(11) . . ? N3B Eu1 N1B 107.7(17) . . ? N3A Eu1 N1B 10.8(6) . . ? N5 Eu1 N4B 105.8(3) . . ? N1A Eu1 N4B 63.7(4) . . ? N3B Eu1 N4B 69.2(7) . . ? N3A Eu1 N4B 94.6(4) . . ? N1B Eu1 N4B 87.6(9) . . ? N5 Eu1 N2A 105.26(14) . . ? N1A Eu1 N2A 70.2(2) . . ? N3B Eu1 N2A 64.9(6) . . ? N3A Eu1 N2A 90.21(18) . . ? N1B Eu1 N2A 101.0(5) . . ? N4B Eu1 N2A 133.8(4) . . ? N5 Eu1 N4A 106.08(14) . . ? N1A Eu1 N4A 87.4(2) . . ? N3B Eu1 N4A 94.2(6) . . ? N3A Eu1 N4A 70.89(18) . . ? N1B Eu1 N4A 61.6(6) . . ? N4B Eu1 N4A 31.0(4) . . ? N2A Eu1 N4A 148.58(16) . . ? N5 Eu1 N2B 106.3(3) . . ? N1A Eu1 N2B 96.3(5) . . ? N3B Eu1 N2B 93.5(10) . . ? N3A Eu1 N2B 61.9(3) . . ? N1B Eu1 N2B 71.6(6) . . ? N4B Eu1 N2B 147.9(5) . . ? N2A Eu1 N2B 35.8(3) . . ? N4A Eu1 N2B 132.7(3) . . ? N5 Eu1 C13B 131.5(6) . . ? N1A Eu1 C13B 18.0(4) . . ? N3B Eu1 C13B 24.5(4) . . ? N3A Eu1 C13B 94.6(6) . . ? N1B Eu1 C13B 95.7(11) . . ? N4B Eu1 C13B 46.1(4) . . ? N2A Eu1 C13B 87.8(3) . . ? N4A Eu1 C13B 69.7(4) . . ? N2B Eu1 C13B 110.4(5) . . ? N5 Eu1 C4B 127.4(7) . . ? N1A Eu1 C4B 99.8(9) . . ? N3B Eu1 C4B 102.7(17) . . ? N3A Eu1 C4B 14.7(4) . . ? N1B Eu1 C4B 24.6(5) . . ? N4B Eu1 C4B 108.6(6) . . ? N2A Eu1 C4B 77.2(4) . . ? N4A Eu1 C4B 85.6(4) . . ? N2B Eu1 C4B 47.2(4) . . ? C13B Eu1 C4B 100.8(9) . . ? N5 Eu1 C13A 131.3(2) . . ? N1A Eu1 C13A 92.6(5) . . ? N3B Eu1 C13A 99.0(13) . . ? N3A Eu1 C13A 23.53(14) . . ? N1B Eu1 C13A 16.0(9) . . ? N4B Eu1 C13A 71.8(4) . . ? N2A Eu1 C13A 109.96(17) . . ? N4A Eu1 C13A 47.55(15) . . ? N2B Eu1 C13A 85.1(3) . . ? C13B Eu1 C13A 82.9(6) . . ? C4B Eu1 C13A 38.2(4) . . ? Si1 N5 Si2 125.0(2) . . ? Si1 N5 Eu1 117.57(18) . . ? Si2 N5 Eu1 117.43(18) . . ? C4A N1A C1A 105.2(8) . . ? C4A N1A Eu1 114.5(6) . . ? C1A N1A Eu1 140.3(6) . . ? C5A N2A C6A 118.9(5) . . ? C5A N2A Eu1 111.9(4) . . ? C6A N2A Eu1 129.2(4) . . ? C10A N3A C13A 106.5(7) . . ? C10A N3A Eu1 140.6(5) . . ? C13A N3A Eu1 112.6(4) . . ? C14A N4A C15A 119.7(5) . . ? C14A N4A Eu1 111.1(4) . . ? C15A N4A Eu1 129.0(4) . . ? C1B N1B C4B 102(2) . . ? C1B N1B Eu1 143(2) . . ? C4B N1B Eu1 108.5(17) . . ? C5B N2B C6B 121.6(14) . . ? C5B N2B Eu1 112.6(11) . . ? C6B N2B Eu1 125.7(9) . . ? C13B N3B C10B 107.0(11) . . ? C13B N3B Eu1 109.2(19) . . ? C10B N3B Eu1 134(3) . . ? C14B N4B C15B 115.0(16) . . ? C14B N4B Eu1 117.3(12) . . ? C15B N4B Eu1 127.7(13) . . ? N5 Si1 C19 107.1(2) . . ? N5 Si1 C21 113.7(3) . . ? C19 Si1 C21 106.2(4) . . ? N5 Si1 C20 114.6(3) . . ? C19 Si1 C20 107.4(3) . . ? C21 Si1 C20 107.4(4) . . ? N5 Si1 Eu1 36.11(12) . . ? C19 Si1 Eu1 70.97(18) . . ? C21 Si1 Eu1 123.8(3) . . ? C20 Si1 Eu1 127.5(2) . . ? N5 Si2 C23 115.2(3) . . ? N5 Si2 C22 107.6(2) . . ? C23 Si2 C22 107.2(4) . . ? N5 Si2 C24 114.0(3) . . ? C23 Si2 C24 105.6(5) . . ? C22 Si2 C24 106.9(4) . . ? N5 Si2 Eu1 36.04(12) . . ? C23 Si2 Eu1 127.8(3) . . ? C22 Si2 Eu1 71.6(2) . . ? C24 Si2 Eu1 125.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1A C1A C2A C3A 3.7(12) . . . . ? C1A C2A C3A C4A -0.6(9) . . . . ? C2A C3A C4A N1A -2.7(15) . . . . ? C2A C3A C4A C5A -176.0(11) . . . . ? C2A C3A C4A Eu1 -9(2) . . . . ? N1A C4A C5A N2A 4.3(18) . . . . ? C3A C4A C5A N2A 177.1(9) . . . . ? Eu1 C4A C5A N2A 2.5(7) . . . . ? N1A C4A C5A Eu1 1.8(13) . . . . ? C3A C4A C5A Eu1 174.6(13) . . . . ? N3A C10A C11A C12A 0.9(11) . . . . ? C10A C11A C12A C13A 0.7(10) . . . . ? C11A C12A C13A N3A -2.1(10) . . . . ? C11A C12A C13A C14A -180.0(9) . . . . ? C11A C12A C13A Eu1 -13.6(16) . . . . ? N3A C13A C14A N4A 1.3(13) . . . . ? C12A C13A C14A N4A 178.9(8) . . . . ? Eu1 C13A C14A N4A 5.5(6) . . . . ? N3A C13A C14A Eu1 -4.2(8) . . . . ? C12A C13A C14A Eu1 173.5(10) . . . . ? N1B C1B C2B C3B 9(4) . . . . ? C1B C2B C3B C4B -1(3) . . . . ? C2B C3B C4B N1B -8(4) . . . . ? C2B C3B C4B C5B 171(3) . . . . ? C2B C3B C4B Eu1 11(8) . . . . ? N1B C4B C5B N2B 4(5) . . . . ? C3B C4B C5B N2B -175(3) . . . . ? Eu1 C4B C5B N2B -2(2) . . . . ? N1B C4B C5B Eu1 6(4) . . . . ? C3B C4B C5B Eu1 -173(4) . . . . ? N3B C10B C11B C12B 11(5) . . . . ? C10B C11B C12B C13B 4(4) . . . . ? C11B C12B C13B N3B -18(4) . . . . ? C11B C12B C13B C14B -173(3) . . . . ? C11B C12B C13B Eu1 -12(6) . . . . ? N3B C13B C14B N4B 22(5) . . . . ? C12B C13B C14B N4B 173(3) . . . . ? Eu1 C13B C14B N4B 1.7(17) . . . . ? N3B C13B C14B Eu1 20(4) . . . . ? C12B C13B C14B Eu1 171(3) . . . . ? N3B C13B Eu1 N5 -88(4) . . . . ? C12B C13B Eu1 N5 -96(4) . . . . ? C14B C13B Eu1 N5 68.4(15) . . . . ? N3B C13B Eu1 N1A 9(5) . . . . ? C12B C13B Eu1 N1A 1(4) . . . . ? C14B C13B Eu1 N1A 165(3) . . . . ? C12B C13B Eu1 N3B -8(5) . . . . ? C14B C13B Eu1 N3B 157(4) . . . . ? N3B C13B Eu1 N3A 110(4) . . . . ? C12B C13B Eu1 N3A 103(4) . . . . ? C14B C13B Eu1 N3A -93.1(14) . . . . ? N3B C13B Eu1 N1B 121(4) . . . . ? C12B C13B Eu1 N1B 114(4) . . . . ? C14B C13B Eu1 N1B -82.3(15) . . . . ? N3B C13B Eu1 N4B -158(4) . . . . ? C12B C13B Eu1 N4B -165(5) . . . . ? C14B C13B Eu1 N4B -1.2(11) . . . . ? N3B C13B Eu1 N2A 20(4) . . . . ? C12B C13B Eu1 N2A 13(4) . . . . ? C14B C13B Eu1 N2A 176.9(14) . . . . ? N3B C13B Eu1 N4A 178(4) . . . . ? C12B C13B Eu1 N4A 170(5) . . . . ? C14B C13B Eu1 N4A -25.4(13) . . . . ? N3B C13B Eu1 N2B 49(4) . . . . ? C12B C13B Eu1 N2B 41(5) . . . . ? C14B C13B Eu1 N2B -154.8(13) . . . . ? N3B C13B Eu1 C4B 97(4) . . . . ? C12B C13B Eu1 C4B 89(4) . . . . ? C14B C13B Eu1 C4B -106.6(14) . . . . ? N3B C13B Eu1 C13A 131(4) . . . . ? C12B C13B Eu1 C13A 123(4) . . . . ? C14B C13B Eu1 C13A -72.7(14) . . . . ? N1B C4B Eu1 N5 -95(3) . . . . ? C5B C4B Eu1 N5 78.2(18) . . . . ? C3B C4B Eu1 N5 -119(7) . . . . ? N1B C4B Eu1 N1A 98(3) . . . . ? C5B C4B Eu1 N1A -88.3(17) . . . . ? C3B C4B Eu1 N1A 74(7) . . . . ? N1B C4B Eu1 N3B 105(3) . . . . ? C5B C4B Eu1 N3B -81.6(18) . . . . ? C3B C4B Eu1 N3B 81(7) . . . . ? N1B C4B Eu1 N3A 14(3) . . . . ? C5B C4B Eu1 N3A -173(4) . . . . ? C3B C4B Eu1 N3A -10(5) . . . . ? C5B C4B Eu1 N1B 173(4) . . . . ? C3B C4B Eu1 N1B -24(6) . . . . ? N1B C4B Eu1 N4B 33(3) . . . . ? C5B C4B Eu1 N4B -153.7(16) . . . . ? C3B C4B Eu1 N4B 9(7) . . . . ? N1B C4B Eu1 N2A 165(3) . . . . ? C5B C4B Eu1 N2A -21.4(16) . . . . ? C3B C4B Eu1 N2A 141(7) . . . . ? N1B C4B Eu1 N4A 12(3) . . . . ? C5B C4B Eu1 N4A -174.9(18) . . . . ? C3B C4B Eu1 N4A -13(7) . . . . ? N1B C4B Eu1 N2B -172(3) . . . . ? C5B C4B Eu1 N2B 1.3(12) . . . . ? C3B C4B Eu1 N2B 164(7) . . . . ? N1B C4B Eu1 C13B 80(3) . . . . ? C5B C4B Eu1 C13B -106.6(17) . . . . ? C3B C4B Eu1 C13B 56(7) . . . . ? N1B C4B Eu1 C13A 17(2) . . . . ? C5B C4B Eu1 C13A -170(3) . . . . ? C3B C4B Eu1 C13A -8(6) . . . . ? N3A C13A Eu1 N5 99.3(7) . . . . ? C12A C13A Eu1 N5 115.1(12) . . . . ? C14A C13A Eu1 N5 -75.5(5) . . . . ? N3A C13A Eu1 N1A -104.3(8) . . . . ? C12A C13A Eu1 N1A -88.5(13) . . . . ? C14A C13A Eu1 N1A 80.9(5) . . . . ? N3A C13A Eu1 N3B -100.9(11) . . . . ? C12A C13A Eu1 N3B -85.1(16) . . . . ? C14A C13A Eu1 N3B 84.2(10) . . . . ? C12A C13A Eu1 N3A 15.8(12) . . . . ? C14A C13A Eu1 N3A -174.9(10) . . . . ? N3A C13A Eu1 N1B 24(3) . . . . ? C12A C13A Eu1 N1B 39(3) . . . . ? C14A C13A Eu1 N1B -151(3) . . . . ? N3A C13A Eu1 N4B -165.4(8) . . . . ? C12A C13A Eu1 N4B -149.7(14) . . . . ? C14A C13A Eu1 N4B 19.7(5) . . . . ? N3A C13A Eu1 N2A -34.4(7) . . . . ? C12A C13A Eu1 N2A -18.7(13) . . . . ? C14A C13A Eu1 N2A 150.7(4) . . . . ? N3A C13A Eu1 N4A 171.7(8) . . . . ? C12A C13A Eu1 N4A -172.6(14) . . . . ? C14A C13A Eu1 N4A -3.2(4) . . . . ? N3A C13A Eu1 N2B -8.1(8) . . . . ? C12A C13A Eu1 N2B 7.7(13) . . . . ? C14A C13A Eu1 N2B 177.0(6) . . . . ? N3A C13A Eu1 C13B -119.4(8) . . . . ? C12A C13A Eu1 C13B -103.7(13) . . . . ? C14A C13A Eu1 C13B 65.7(6) . . . . ? N3A C13A Eu1 C4B -1.7(13) . . . . ? C12A C13A Eu1 C4B 14.0(16) . . . . ? C14A C13A Eu1 C4B -176.6(13) . . . . ? N1A Eu1 N5 Si1 7.0(4) . . . . ? N3B Eu1 N5 Si1 0.1(8) . . . . ? N3A Eu1 N5 Si1 -173.7(2) . . . . ? N1B Eu1 N5 Si1 174.2(8) . . . . ? N4B Eu1 N5 Si1 75.6(4) . . . . ? N2A Eu1 N5 Si1 -69.8(2) . . . . ? N4A Eu1 N5 Si1 107.9(2) . . . . ? N2B Eu1 N5 Si1 -107.1(4) . . . . ? C13B Eu1 N5 Si1 31.0(5) . . . . ? C4B Eu1 N5 Si1 -155.2(5) . . . . ? C13A Eu1 N5 Si1 154.9(2) . . . . ? N1A Eu1 N5 Si2 -172.4(3) . . . . ? N3B Eu1 N5 Si2 -179.4(7) . . . . ? N3A Eu1 N5 Si2 6.9(3) . . . . ? N1B Eu1 N5 Si2 -5.3(8) . . . . ? N4B Eu1 N5 Si2 -103.8(4) . . . . ? N2A Eu1 N5 Si2 110.8(2) . . . . ? N4A Eu1 N5 Si2 -71.5(2) . . . . ? N2B Eu1 N5 Si2 73.5(4) . . . . ? C13B Eu1 N5 Si2 -148.4(5) . . . . ? C4B Eu1 N5 Si2 25.4(5) . . . . ? C13A Eu1 N5 Si2 -24.5(3) . . . . ? C5A C4A N1A C1A 178.7(11) . . . . ? C3A C4A N1A C1A 4.9(18) . . . . ? Eu1 C4A N1A C1A -179(2) . . . . ? C5A C4A N1A Eu1 -2.6(19) . . . . ? C3A C4A N1A Eu1 -176.4(9) . . . . ? C2A C1A N1A C4A -5.2(17) . . . . ? C2A C1A N1A Eu1 176.6(15) . . . . ? N5 Eu1 N1A C4A -92.6(13) . . . . ? N3B Eu1 N1A C4A -41(13) . . . . ? N3A Eu1 N1A C4A 87.9(13) . . . . ? N1B Eu1 N1A C4A 98.0(14) . . . . ? N4B Eu1 N1A C4A 179.1(16) . . . . ? N2A Eu1 N1A C4A 0.6(12) . . . . ? N4A Eu1 N1A C4A 158.2(13) . . . . ? N2B Eu1 N1A C4A 25.5(14) . . . . ? C13B Eu1 N1A C4A 168(3) . . . . ? C4B Eu1 N1A C4A 73.1(13) . . . . ? C13A Eu1 N1A C4A 110.9(13) . . . . ? N5 Eu1 N1A C1A 85.4(19) . . . . ? N3B Eu1 N1A C1A 137(16) . . . . ? N3A Eu1 N1A C1A -94(2) . . . . ? N1B Eu1 N1A C1A -84(2) . . . . ? N4B Eu1 N1A C1A -2.9(18) . . . . ? N2A Eu1 N1A C1A 179(2) . . . . ? N4A Eu1 N1A C1A -24(2) . . . . ? N2B Eu1 N1A C1A -156.5(19) . . . . ? C13B Eu1 N1A C1A -14(2) . . . . ? C4B Eu1 N1A C1A -109(2) . . . . ? C13A Eu1 N1A C1A -71(2) . . . . ? C4A C5A N2A C6A 178.6(8) . . . . ? Eu1 C5A N2A C6A -178.0(6) . . . . ? C4A C5A N2A Eu1 -3.4(9) . . . . ? C9A C6A N2A C5A 175.4(6) . . . . ? C8A C6A N2A C5A -69.2(7) . . . . ? C7A C6A N2A C5A 54.0(10) . . . . ? C9A C6A N2A Eu1 -2.3(7) . . . . ? C8A C6A N2A Eu1 113.1(6) . . . . ? C7A C6A N2A Eu1 -123.6(9) . . . . ? N5 Eu1 N2A C5A 130.1(4) . . . . ? N1A Eu1 N2A C5A 1.4(6) . . . . ? N3B Eu1 N2A C5A 6.7(17) . . . . ? N3A Eu1 N2A C5A -97.1(4) . . . . ? N1B Eu1 N2A C5A -97.9(11) . . . . ? N4B Eu1 N2A C5A -0.6(7) . . . . ? N4A Eu1 N2A C5A -45.6(5) . . . . ? N2B Eu1 N2A C5A -133.1(7) . . . . ? C13B Eu1 N2A C5A -2.5(7) . . . . ? C4B Eu1 N2A C5A -104.2(8) . . . . ? C13A Eu1 N2A C5A -84.1(4) . . . . ? N5 Eu1 N2A C6A -52.1(5) . . . . ? N1A Eu1 N2A C6A 179.1(7) . . . . ? N3B Eu1 N2A C6A -175.6(17) . . . . ? N3A Eu1 N2A C6A 80.6(5) . . . . ? N1B Eu1 N2A C6A 79.9(11) . . . . ? N4B Eu1 N2A C6A 177.2(6) . . . . ? N4A Eu1 N2A C6A 132.2(5) . . . . ? N2B Eu1 N2A C6A 44.7(6) . . . . ? C13B Eu1 N2A C6A 175.3(7) . . . . ? C4B Eu1 N2A C6A 73.6(8) . . . . ? C13A Eu1 N2A C6A 93.7(5) . . . . ? C11A C10A N3A C13A -2.2(12) . . . . ? C11A C10A N3A Eu1 170.2(9) . . . . ? C12A C13A N3A C10A 2.6(11) . . . . ? C14A C13A N3A C10A -179.3(9) . . . . ? Eu1 C13A N3A C10A 174.8(12) . . . . ? C12A C13A N3A Eu1 -172.2(6) . . . . ? C14A C13A N3A Eu1 5.9(11) . . . . ? N5 Eu1 N3A C10A 86.3(13) . . . . ? N1A Eu1 N3A C10A -94.2(13) . . . . ? N3B Eu1 N3A C10A -88.5(14) . . . . ? N1B Eu1 N3A C10A 152(7) . . . . ? N4B Eu1 N3A C10A -158.3(13) . . . . ? N2A Eu1 N3A C10A -24.2(13) . . . . ? N4A Eu1 N3A C10A -178.7(13) . . . . ? N2B Eu1 N3A C10A -1.3(12) . . . . ? C13B Eu1 N3A C10A -112.0(13) . . . . ? C4B Eu1 N3A C10A 4(3) . . . . ? C13A Eu1 N3A C10A -172.1(18) . . . . ? N5 Eu1 N3A C13A -101.6(7) . . . . ? N1A Eu1 N3A C13A 77.9(7) . . . . ? N3B Eu1 N3A C13A 83.6(9) . . . . ? N1B Eu1 N3A C13A -36(6) . . . . ? N4B Eu1 N3A C13A 13.9(8) . . . . ? N2A Eu1 N3A C13A 147.9(7) . . . . ? N4A Eu1 N3A C13A -6.5(6) . . . . ? N2B Eu1 N3A C13A 170.8(9) . . . . ? C13B Eu1 N3A C13A 60.1(7) . . . . ? C4B Eu1 N3A C13A 176(3) . . . . ? C13A C14A N4A C15A 176.7(7) . . . . ? Eu1 C14A N4A C15A -176.0(7) . . . . ? C13A C14A N4A Eu1 -7.3(8) . . . . ? C18A C15A N4A C14A -69.0(8) . . . . ? C16A C15A N4A C14A 169.4(6) . . . . ? C17A C15A N4A C14A 51.3(8) . . . . ? C18A C15A N4A Eu1 115.8(6) . . . . ? C16A C15A N4A Eu1 -5.8(8) . . . . ? C17A C15A N4A Eu1 -123.9(6) . . . . ? N5 Eu1 N4A C14A 135.5(4) . . . . ? N1A Eu1 N4A C14A -92.3(6) . . . . ? N3B Eu1 N4A C14A -94.7(16) . . . . ? N3A Eu1 N4A C14A 7.2(5) . . . . ? N1B Eu1 N4A C14A 13.2(11) . . . . ? N4B Eu1 N4A C14A -130.5(8) . . . . ? N2A Eu1 N4A C14A -48.8(6) . . . . ? N2B Eu1 N4A C14A 4.0(7) . . . . ? C13B Eu1 N4A C14A -95.5(7) . . . . ? C4B Eu1 N4A C14A 7.8(8) . . . . ? C13A Eu1 N4A C14A 3.7(4) . . . . ? N5 Eu1 N4A C15A -49.0(5) . . . . ? N1A Eu1 N4A C15A 83.2(7) . . . . ? N3B Eu1 N4A C15A 80.8(16) . . . . ? N3A Eu1 N4A C15A -177.3(6) . . . . ? N1B Eu1 N4A C15A -171.3(12) . . . . ? N4B Eu1 N4A C15A 44.9(8) . . . . ? N2A Eu1 N4A C15A 126.7(5) . . . . ? N2B Eu1 N4A C15A 179.5(6) . . . . ? C13B Eu1 N4A C15A 80.0(8) . . . . ? C4B Eu1 N4A C15A -176.7(9) . . . . ? C13A Eu1 N4A C15A 179.2(6) . . . . ? C2B C1B N1B C4B -13(4) . . . . ? C2B C1B N1B Eu1 -158(3) . . . . ? C5B C4B N1B C1B -166(4) . . . . ? C3B C4B N1B C1B 13(4) . . . . ? Eu1 C4B N1B C1B -158(4) . . . . ? C5B C4B N1B Eu1 -8(5) . . . . ? C3B C4B N1B Eu1 171(3) . . . . ? N5 Eu1 N1B C1B -114(4) . . . . ? N1A Eu1 N1B C1B 56(4) . . . . ? N3B Eu1 N1B C1B 61(4) . . . . ? N3A Eu1 N1B C1B 124(9) . . . . ? N4B Eu1 N1B C1B -6(4) . . . . ? N2A Eu1 N1B C1B 128(4) . . . . ? N4A Eu1 N1B C1B -24(4) . . . . ? N2B Eu1 N1B C1B 149(4) . . . . ? C13B Eu1 N1B C1B 39(4) . . . . ? C4B Eu1 N1B C1B 143(6) . . . . ? C13A Eu1 N1B C1B 2(3) . . . . ? N5 Eu1 N1B C4B 103(3) . . . . ? N1A Eu1 N1B C4B -87(3) . . . . ? N3B Eu1 N1B C4B -82(3) . . . . ? N3A Eu1 N1B C4B -19(5) . . . . ? N4B Eu1 N1B C4B -149(3) . . . . ? N2A Eu1 N1B C4B -15(3) . . . . ? N4A Eu1 N1B C4B -167(3) . . . . ? N2B Eu1 N1B C4B 6(3) . . . . ? C13B Eu1 N1B C4B -104(3) . . . . ? C13A Eu1 N1B C4B -140(5) . . . . ? C4B C5B N2B C6B -175(2) . . . . ? Eu1 C5B N2B C6B -178(2) . . . . ? C4B C5B N2B Eu1 3(3) . . . . ? C7B C6B N2B C5B -55(2) . . . . ? C9B C6B N2B C5B -179.1(18) . . . . ? C8B C6B N2B C5B 61.6(18) . . . . ? C7B C6B N2B Eu1 127.5(14) . . . . ? C9B C6B N2B Eu1 4(2) . . . . ? C8B C6B N2B Eu1 -115.8(12) . . . . ? N5 Eu1 N2B C5B -127.8(12) . . . . ? N1A Eu1 N2B C5B 96.0(13) . . . . ? N3B Eu1 N2B C5B 102.6(17) . . . . ? N3A Eu1 N2B C5B 0.2(11) . . . . ? N1B Eu1 N2B C5B -4.9(15) . . . . ? N4B Eu1 N2B C5B 47.4(17) . . . . ? N2A Eu1 N2B C5B 138.5(15) . . . . ? N4A Eu1 N2B C5B 3.7(14) . . . . ? C13B Eu1 N2B C5B 84.4(13) . . . . ? C4B Eu1 N2B C5B -1.5(14) . . . . ? C13A Eu1 N2B C5B 3.9(12) . . . . ? N5 Eu1 N2B C6B 49.8(13) . . . . ? N1A Eu1 N2B C6B -86.4(14) . . . . ? N3B Eu1 N2B C6B -79.8(18) . . . . ? N3A Eu1 N2B C6B 177.8(15) . . . . ? N1B Eu1 N2B C6B 172.7(17) . . . . ? N4B Eu1 N2B C6B -135.1(13) . . . . ? N2A Eu1 N2B C6B -43.9(11) . . . . ? N4A Eu1 N2B C6B -178.8(11) . . . . ? C13B Eu1 N2B C6B -98.0(14) . . . . ? C4B Eu1 N2B C6B 176.1(18) . . . . ? C13A Eu1 N2B C6B -178.5(13) . . . . ? C12B C13B N3B C10B 25(6) . . . . ? C14B C13B N3B C10B -180(3) . . . . ? Eu1 C13B N3B C10B -151(7) . . . . ? C12B C13B N3B Eu1 176(2) . . . . ? C14B C13B N3B Eu1 -28(5) . . . . ? C11B C10B N3B C13B -23(6) . . . . ? C11B C10B N3B Eu1 -164(4) . . . . ? N5 Eu1 N3B C13B 112(3) . . . . ? N1A Eu1 N3B C13B -22(11) . . . . ? N3A Eu1 N3B C13B -73(4) . . . . ? N1B Eu1 N3B C13B -63(4) . . . . ? N4B Eu1 N3B C13B 17(3) . . . . ? N2A Eu1 N3B C13B -157(4) . . . . ? N4A Eu1 N3B C13B -2(4) . . . . ? N2B Eu1 N3B C13B -135(3) . . . . ? C4B Eu1 N3B C13B -88(4) . . . . ? C13A Eu1 N3B C13B -50(4) . . . . ? N5 Eu1 N3B C10B -108(5) . . . . ? N1A Eu1 N3B C10B 119(18) . . . . ? N3A Eu1 N3B C10B 67(5) . . . . ? N1B Eu1 N3B C10B 77(5) . . . . ? N4B Eu1 N3B C10B 157(6) . . . . ? N2A Eu1 N3B C10B -17(4) . . . . ? N4A Eu1 N3B C10B 138(5) . . . . ? N2B Eu1 N3B C10B 5(5) . . . . ? C13B Eu1 N3B C10B 140(8) . . . . ? C4B Eu1 N3B C10B 52(5) . . . . ? C13A Eu1 N3B C10B 91(5) . . . . ? C13B C14B N4B C15B 179.0(19) . . . . ? Eu1 C14B N4B C15B -179(2) . . . . ? C13B C14B N4B Eu1 -2(2) . . . . ? C17B C15B N4B C14B -59(3) . . . . ? C16B C15B N4B C14B -179(2) . . . . ? C18B C15B N4B C14B 75(3) . . . . ? C17B C15B N4B Eu1 123(2) . . . . ? C16B C15B N4B Eu1 3(3) . . . . ? C18B C15B N4B Eu1 -104(2) . . . . ? N5 Eu1 N4B C14B -131.8(13) . . . . ? N1A Eu1 N4B C14B -3.3(14) . . . . ? N3B Eu1 N4B C14B -8(2) . . . . ? N3A Eu1 N4B C14B 93.4(14) . . . . ? N1B Eu1 N4B C14B 101.7(16) . . . . ? N2A Eu1 N4B C14B -1.3(16) . . . . ? N4A Eu1 N4B C14B 133.1(17) . . . . ? N2B Eu1 N4B C14B 53.0(18) . . . . ? C13B Eu1 N4B C14B 1.4(14) . . . . ? C4B Eu1 N4B C14B 88.7(15) . . . . ? C13A Eu1 N4B C14B 99.2(14) . . . . ? N5 Eu1 N4B C15B 46.5(15) . . . . ? N1A Eu1 N4B C15B 175.0(17) . . . . ? N3B Eu1 N4B C15B 170(2) . . . . ? N3A Eu1 N4B C15B -88.3(15) . . . . ? N1B Eu1 N4B C15B -80.0(17) . . . . ? N2A Eu1 N4B C15B 177.0(13) . . . . ? N4A Eu1 N4B C15B -48.6(14) . . . . ? N2B Eu1 N4B C15B -128.7(14) . . . . ? C13B Eu1 N4B C15B 179.7(19) . . . . ? C4B Eu1 N4B C15B -93.0(16) . . . . ? C13A Eu1 N4B C15B -82.5(15) . . . . ? Si2 N5 Si1 C19 177.8(3) . . . . ? Eu1 N5 Si1 C19 -1.6(4) . . . . ? Si2 N5 Si1 C21 -65.3(4) . . . . ? Eu1 N5 Si1 C21 115.4(3) . . . . ? Si2 N5 Si1 C20 58.8(4) . . . . ? Eu1 N5 Si1 C20 -120.6(3) . . . . ? Si2 N5 Si1 Eu1 179.4(4) . . . . ? N1A Eu1 Si1 N5 -174.6(3) . . . . ? N3B Eu1 Si1 N5 -180.0(6) . . . . ? N3A Eu1 Si1 N5 12.2(4) . . . . ? N1B Eu1 Si1 N5 -10.0(14) . . . . ? N4B Eu1 Si1 N5 -109.7(4) . . . . ? N2A Eu1 Si1 N5 114.7(2) . . . . ? N4A Eu1 Si1 N5 -81.2(3) . . . . ? N2B Eu1 Si1 N5 82.1(4) . . . . ? C13B Eu1 Si1 N5 -156.0(4) . . . . ? C4B Eu1 Si1 N5 41.5(10) . . . . ? C13A Eu1 Si1 N5 -45.1(4) . . . . ? N5 Eu1 Si1 C19 178.4(4) . . . . ? N1A Eu1 Si1 C19 3.8(3) . . . . ? N3B Eu1 Si1 C19 -1.6(6) . . . . ? N3A Eu1 Si1 C19 -169.4(4) . . . . ? N1B Eu1 Si1 C19 168.4(14) . . . . ? N4B Eu1 Si1 C19 68.6(5) . . . . ? N2A Eu1 Si1 C19 -66.9(3) . . . . ? N4A Eu1 Si1 C19 97.2(3) . . . . ? N2B Eu1 Si1 C19 -99.5(4) . . . . ? C13B Eu1 Si1 C19 22.4(4) . . . . ? C4B Eu1 Si1 C19 -140.1(10) . . . . ? C13A Eu1 Si1 C19 133.3(4) . . . . ? N5 Eu1 Si1 C21 -84.5(4) . . . . ? N1A Eu1 Si1 C21 101.0(4) . . . . ? N3B Eu1 Si1 C21 95.6(7) . . . . ? N3A Eu1 Si1 C21 -72.3(5) . . . . ? N1B Eu1 Si1 C21 -94.5(15) . . . . ? N4B Eu1 Si1 C21 165.8(5) . . . . ? N2A Eu1 Si1 C21 30.2(3) . . . . ? N4A Eu1 Si1 C21 -165.6(3) . . . . ? N2B Eu1 Si1 C21 -2.4(5) . . . . ? C13B Eu1 Si1 C21 119.5(4) . . . . ? C4B Eu1 Si1 C21 -42.9(10) . . . . ? C13A Eu1 Si1 C21 -129.5(4) . . . . ? N5 Eu1 Si1 C20 80.6(4) . . . . ? N1A Eu1 Si1 C20 -93.9(4) . . . . ? N3B Eu1 Si1 C20 -99.3(7) . . . . ? N3A Eu1 Si1 C20 92.8(5) . . . . ? N1B Eu1 Si1 C20 70.6(15) . . . . ? N4B Eu1 Si1 C20 -29.1(5) . . . . ? N2A Eu1 Si1 C20 -164.7(3) . . . . ? N4A Eu1 Si1 C20 -0.5(3) . . . . ? N2B Eu1 Si1 C20 162.7(5) . . . . ? C13B Eu1 Si1 C20 -75.4(4) . . . . ? C4B Eu1 Si1 C20 122.2(10) . . . . ? C13A Eu1 Si1 C20 35.6(4) . . . . ? Si1 N5 Si2 C23 -59.1(5) . . . . ? Eu1 N5 Si2 C23 120.3(4) . . . . ? Si1 N5 Si2 C22 -178.5(4) . . . . ? Eu1 N5 Si2 C22 0.9(4) . . . . ? Si1 N5 Si2 C24 63.2(5) . . . . ? Eu1 N5 Si2 C24 -117.4(4) . . . . ? Si1 N5 Si2 Eu1 -179.4(4) . . . . ? N1A Eu1 Si2 N5 14.8(5) . . . . ? N3B Eu1 Si2 N5 1.1(13) . . . . ? N3A Eu1 Si2 N5 -174.6(3) . . . . ? N1B Eu1 Si2 N5 175.7(7) . . . . ? N4B Eu1 Si2 N5 84.8(4) . . . . ? N2A Eu1 Si2 N5 -78.2(2) . . . . ? N4A Eu1 Si2 N5 113.5(3) . . . . ? N2B Eu1 Si2 N5 -111.8(4) . . . . ? C13B Eu1 Si2 N5 55.1(10) . . . . ? C4B Eu1 Si2 N5 -159.5(4) . . . . ? C13A Eu1 Si2 N5 161.0(2) . . . . ? N5 Eu1 Si2 C23 -81.3(4) . . . . ? N1A Eu1 Si2 C23 -66.5(6) . . . . ? N3B Eu1 Si2 C23 -80.2(13) . . . . ? N3A Eu1 Si2 C23 104.1(4) . . . . ? N1B Eu1 Si2 C23 94.4(7) . . . . ? N4B Eu1 Si2 C23 3.5(5) . . . . ? N2A Eu1 Si2 C23 -159.5(4) . . . . ? N4A Eu1 Si2 C23 32.2(4) . . . . ? N2B Eu1 Si2 C23 166.8(5) . . . . ? C13B Eu1 Si2 C23 -26.2(10) . . . . ? C4B Eu1 Si2 C23 119.1(5) . . . . ? C13A Eu1 Si2 C23 79.7(4) . . . . ? N5 Eu1 Si2 C22 -179.1(4) . . . . ? N1A Eu1 Si2 C22 -164.3(5) . . . . ? N3B Eu1 Si2 C22 -178.0(13) . . . . ? N3A Eu1 Si2 C22 6.3(3) . . . . ? N1B Eu1 Si2 C22 -3.4(7) . . . . ? N4B Eu1 Si2 C22 -94.3(5) . . . . ? N2A Eu1 Si2 C22 102.7(3) . . . . ? N4A Eu1 Si2 C22 -65.6(3) . . . . ? N2B Eu1 Si2 C22 69.1(4) . . . . ? C13B Eu1 Si2 C22 -124.0(10) . . . . ? C4B Eu1 Si2 C22 21.4(5) . . . . ? C13A Eu1 Si2 C22 -18.1(3) . . . . ? N5 Eu1 Si2 C24 82.9(4) . . . . ? N1A Eu1 Si2 C24 97.7(6) . . . . ? N3B Eu1 Si2 C24 84.0(13) . . . . ? N3A Eu1 Si2 C24 -91.7(4) . . . . ? N1B Eu1 Si2 C24 -101.4(7) . . . . ? N4B Eu1 Si2 C24 167.7(5) . . . . ? N2A Eu1 Si2 C24 4.7(4) . . . . ? N4A Eu1 Si2 C24 -163.6(4) . . . . ? N2B Eu1 Si2 C24 -28.9(5) . . . . ? C13B Eu1 Si2 C24 138.0(10) . . . . ? C4B Eu1 Si2 C24 -76.6(5) . . . . ? C13A Eu1 Si2 C24 -116.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.788 _refine_diff_density_min -0.914 _refine_diff_density_rms 0.080 data_4a _database_code_depnum_ccdc_archive 'CCDC 896990' #TrackingRef 'CCDC-896990.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H60 N5 Si2 Y' _chemical_formula_weight 659.94 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.3948(15) _cell_length_b 16.9374(15) _cell_length_c 13.8194(12) _cell_angle_alpha 90.00 _cell_angle_beta 99.0520(10) _cell_angle_gamma 90.00 _cell_volume 3789.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5977 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 1.628 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5550 _exptl_absorpt_correction_T_max 0.7262 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14518 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3726 _reflns_number_gt 3081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+1.9947P] 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 3726 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0920(2) 0.2254(2) 0.0092(2) 0.0872(10) Uani 1 1 d . . . H1A H -0.0713 0.1851 0.0555 0.131 Uiso 1 1 calc R . . H1B H -0.1413 0.2069 -0.0314 0.131 Uiso 1 1 calc R . . H1C H -0.1045 0.2719 0.0437 0.131 Uiso 1 1 calc R . . C2 C -0.0086(3) 0.1703(2) -0.1110(3) 0.1213(16) Uani 1 1 d . . . H2A H 0.0083 0.1283 -0.0656 0.182 Uiso 1 1 calc R . . H2B H 0.0350 0.1816 -0.1479 0.182 Uiso 1 1 calc R . . H2C H -0.0572 0.1546 -0.1549 0.182 Uiso 1 1 calc R . . C3 C -0.0619(3) 0.3088(2) -0.1299(2) 0.1005(12) Uani 1 1 d . . . H3A H -0.1086 0.2881 -0.1732 0.151 Uiso 1 1 calc R . . H3B H -0.0198 0.3240 -0.1673 0.151 Uiso 1 1 calc R . . H3C H -0.0787 0.3541 -0.0962 0.151 Uiso 1 1 calc R . . C4 C -0.0275(2) 0.24471(17) -0.0542(2) 0.0767(9) Uani 1 1 d . . . C5 C 0.0502(2) 0.27646(15) 0.0056(2) 0.0651(8) Uani 1 1 d . . . C6 C 0.1257(3) 0.28971(19) -0.0270(3) 0.0891(11) Uani 1 1 d . . . H6 H 0.1388 0.2742 -0.0872 0.107 Uiso 1 1 calc R . . C7 C 0.1767(2) 0.3290(2) 0.0442(3) 0.0848(10) Uani 1 1 d . . . H7 H 0.2304 0.3455 0.0418 0.102 Uiso 1 1 calc R . . C8 C 0.13215(16) 0.33978(15) 0.1219(2) 0.0615(7) Uani 1 1 d . . . C9 C 0.15565(15) 0.38262(14) 0.2080(2) 0.0597(7) Uani 1 1 d . . . H9 H 0.2069 0.4074 0.2167 0.072 Uiso 1 1 calc R . . C10 C 0.13764(15) 0.45181(14) 0.3540(2) 0.0591(6) Uani 1 1 d . . . C11 C 0.1553(2) 0.53026(16) 0.3052(2) 0.0831(9) Uani 1 1 d . . . H11A H 0.2004 0.5233 0.2694 0.125 Uiso 1 1 calc R . . H11B H 0.1693 0.5699 0.3546 0.125 Uiso 1 1 calc R . . H11C H 0.1070 0.5465 0.2610 0.125 Uiso 1 1 calc R . . C12 C 0.2149(2) 0.4248(2) 0.4220(3) 0.0954(11) Uani 1 1 d . . . H12A H 0.2036 0.3763 0.4533 0.143 Uiso 1 1 calc R . . H12B H 0.2310 0.4645 0.4709 0.143 Uiso 1 1 calc R . . H12C H 0.2589 0.4166 0.3847 0.143 Uiso 1 1 calc R . . C13 C 0.0673(2) 0.46606(17) 0.4108(2) 0.0790(9) Uani 1 1 d . . . H13A H 0.0193 0.4830 0.3667 0.118 Uiso 1 1 calc R . . H13B H 0.0830 0.5062 0.4593 0.118 Uiso 1 1 calc R . . H13C H 0.0551 0.4181 0.4425 0.118 Uiso 1 1 calc R . . C14 C 0.1004(2) 0.0758(2) 0.1220(2) 0.0956(11) Uani 1 1 d . . . H14A H 0.0529 0.0445 0.0974 0.143 Uiso 1 1 calc R . . H14B H 0.1492 0.0439 0.1260 0.143 Uiso 1 1 calc R . . H14C H 0.1043 0.1194 0.0787 0.143 Uiso 1 1 calc R . . C15 C 0.18218(17) 0.17954(17) 0.2823(3) 0.0751(8) Uani 1 1 d . . . H15A H 0.1862 0.2162 0.2303 0.113 Uiso 1 1 calc R . . H15B H 0.2315 0.1481 0.2943 0.113 Uiso 1 1 calc R . . H15C H 0.1759 0.2080 0.3407 0.113 Uiso 1 1 calc R . . C16 C 0.1071(2) 0.02700(17) 0.3316(3) 0.0879(10) Uani 1 1 d . . . H16A H 0.1041 0.0441 0.3972 0.132 Uiso 1 1 calc R . . H16B H 0.1605 0.0044 0.3293 0.132 Uiso 1 1 calc R . . H16C H 0.0652 -0.0119 0.3119 0.132 Uiso 1 1 calc R . . N1 N 0.05433(13) 0.30584(11) 0.09825(15) 0.0534(5) Uani 1 1 d . . . N2 N 0.11058(12) 0.39026(11) 0.27704(15) 0.0522(5) Uani 1 1 d . . . N3 N 0.0000 0.16374(14) 0.2500 0.0473(6) Uani 1 2 d S . . Si1 Si 0.09056(5) 0.11373(4) 0.24642(6) 0.0574(2) Uani 1 1 d . . . Y1 Y 0.0000 0.295979(16) 0.2500 0.04165(11) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.107(3) 0.087(2) 0.0642(19) -0.0028(16) 0.0004(18) -0.0190(19) C2 0.204(5) 0.085(2) 0.069(2) -0.0212(19) 0.005(3) 0.037(3) C3 0.141(3) 0.095(3) 0.065(2) 0.0180(18) 0.017(2) 0.033(2) C4 0.123(3) 0.0606(17) 0.0479(16) -0.0013(13) 0.0178(17) 0.0167(17) C5 0.096(2) 0.0494(14) 0.0567(16) 0.0092(12) 0.0330(16) 0.0208(14) C6 0.119(3) 0.081(2) 0.083(2) 0.0073(18) 0.062(2) 0.026(2) C7 0.080(2) 0.082(2) 0.105(3) 0.017(2) 0.055(2) 0.0145(18) C8 0.0611(16) 0.0520(15) 0.0791(19) 0.0145(13) 0.0345(14) 0.0092(12) C9 0.0446(13) 0.0507(14) 0.086(2) 0.0158(14) 0.0177(13) -0.0001(11) C10 0.0532(14) 0.0494(13) 0.0715(17) 0.0038(12) 0.0004(12) -0.0125(11) C11 0.097(2) 0.0527(16) 0.101(2) 0.0048(15) 0.0185(19) -0.0200(16) C12 0.078(2) 0.094(2) 0.104(3) 0.015(2) -0.0183(19) -0.0144(18) C13 0.087(2) 0.0688(18) 0.083(2) -0.0190(16) 0.0212(17) -0.0236(16) C14 0.095(2) 0.104(3) 0.089(2) -0.017(2) 0.0152(19) 0.049(2) C15 0.0560(16) 0.0642(16) 0.107(2) 0.0074(16) 0.0199(16) 0.0078(13) C16 0.090(2) 0.0567(17) 0.112(3) 0.0233(17) 0.0013(19) 0.0116(16) N1 0.0651(13) 0.0458(11) 0.0542(12) 0.0069(9) 0.0245(10) 0.0099(10) N2 0.0441(10) 0.0447(10) 0.0685(13) 0.0074(9) 0.0112(10) -0.0015(8) N3 0.0535(16) 0.0352(13) 0.0539(16) 0.000 0.0110(13) 0.000 Si1 0.0622(4) 0.0427(4) 0.0671(5) 0.0027(3) 0.0097(4) 0.0112(3) Y1 0.04105(17) 0.03492(16) 0.0515(2) 0.000 0.01493(13) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C4 1.512(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C4 1.543(4) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.551(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.504(5) . ? C5 N1 1.365(3) . ? C5 C6 1.401(4) . ? C6 C7 1.360(5) . ? C6 H6 0.9300 . ? C7 C8 1.402(4) . ? C7 H7 0.9300 . ? C8 N1 1.390(3) . ? C8 C9 1.396(4) . ? C9 N2 1.301(3) . ? C9 H9 0.9300 . ? C10 N2 1.505(3) . ? C10 C13 1.513(4) . ? C10 C12 1.524(4) . ? C10 C11 1.538(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 Si1 1.866(3) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 Si1 1.874(3) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 Si1 1.875(3) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N1 Y1 2.4098(19) . ? N2 Y1 2.4007(19) . ? N3 Si1 1.7167(14) 2 ? N3 Si1 1.7168(14) . ? N3 Y1 2.240(2) . ? Y1 N2 2.4007(19) 2 ? Y1 N1 2.4098(19) 2 ? Y1 Si1 3.4291(7) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C1 111.6(2) . . ? C5 C4 C2 110.6(3) . . ? C1 C4 C2 109.5(3) . . ? C5 C4 C3 107.9(3) . . ? C1 C4 C3 109.2(3) . . ? C2 C4 C3 108.0(3) . . ? N1 C5 C6 109.1(3) . . ? N1 C5 C4 124.0(3) . . ? C6 C5 C4 126.5(3) . . ? C7 C6 C5 108.6(3) . . ? C7 C6 H6 125.7 . . ? C5 C6 H6 125.7 . . ? C6 C7 C8 106.4(3) . . ? C6 C7 H7 126.8 . . ? C8 C7 H7 126.8 . . ? N1 C8 C9 122.3(2) . . ? N1 C8 C7 109.6(3) . . ? C9 C8 C7 127.9(3) . . ? N2 C9 C8 124.4(2) . . ? N2 C9 H9 117.8 . . ? C8 C9 H9 117.8 . . ? N2 C10 C13 108.3(2) . . ? N2 C10 C12 110.6(2) . . ? C13 C10 C12 110.8(3) . . ? N2 C10 C11 110.1(2) . . ? C13 C10 C11 107.5(2) . . ? C12 C10 C11 109.5(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C5 N1 C8 106.2(2) . . ? C5 N1 Y1 145.08(18) . . ? C8 N1 Y1 105.99(16) . . ? C9 N2 C10 116.6(2) . . ? C9 N2 Y1 108.77(16) . . ? C10 N2 Y1 134.60(15) . . ? Si1 N3 Si1 120.87(15) 2 . ? Si1 N3 Y1 119.56(8) 2 . ? Si1 N3 Y1 119.56(8) . . ? N3 Si1 C14 113.41(10) . . ? N3 Si1 C15 111.09(12) . . ? C14 Si1 C15 105.47(17) . . ? N3 Si1 C16 114.12(13) . . ? C14 Si1 C16 106.46(16) . . ? C15 Si1 C16 105.61(14) . . ? N3 Y1 N2 131.70(5) . . ? N3 Y1 N2 131.70(5) . 2 ? N2 Y1 N2 96.61(9) . 2 ? N3 Y1 N1 93.97(4) . . ? N2 Y1 N1 73.49(7) . . ? N2 Y1 N1 101.06(7) 2 . ? N3 Y1 N1 93.97(4) . 2 ? N2 Y1 N1 101.06(7) . 2 ? N2 Y1 N1 73.49(7) 2 2 ? N1 Y1 N1 172.05(9) . 2 ? N3 Y1 Si1 25.815(13) . 2 ? N2 Y1 Si1 156.15(5) . 2 ? N2 Y1 Si1 106.44(5) 2 2 ? N1 Y1 Si1 107.17(5) . 2 ? N1 Y1 Si1 80.19(5) 2 2 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C4 C5 N1 -17.9(4) . . . . ? C2 C4 C5 N1 -140.0(3) . . . . ? C3 C4 C5 N1 102.1(3) . . . . ? C1 C4 C5 C6 170.4(3) . . . . ? C2 C4 C5 C6 48.3(4) . . . . ? C3 C4 C5 C6 -69.7(4) . . . . ? N1 C5 C6 C7 -1.4(3) . . . . ? C4 C5 C6 C7 171.4(3) . . . . ? C5 C6 C7 C8 0.3(4) . . . . ? C6 C7 C8 N1 0.9(3) . . . . ? C6 C7 C8 C9 -174.2(3) . . . . ? N1 C8 C9 N2 5.2(4) . . . . ? C7 C8 C9 N2 179.7(3) . . . . ? C6 C5 N1 C8 1.9(3) . . . . ? C4 C5 N1 C8 -171.1(2) . . . . ? C6 C5 N1 Y1 -154.8(2) . . . . ? C4 C5 N1 Y1 32.2(4) . . . . ? C9 C8 N1 C5 173.7(2) . . . . ? C7 C8 N1 C5 -1.7(3) . . . . ? C9 C8 N1 Y1 -19.9(3) . . . . ? C7 C8 N1 Y1 164.65(19) . . . . ? C8 C9 N2 C10 -167.6(2) . . . . ? C8 C9 N2 Y1 13.4(3) . . . . ? C13 C10 N2 C9 165.7(2) . . . . ? C12 C10 N2 C9 -72.7(3) . . . . ? C11 C10 N2 C9 48.4(3) . . . . ? C13 C10 N2 Y1 -15.6(3) . . . . ? C12 C10 N2 Y1 106.0(2) . . . . ? C11 C10 N2 Y1 -132.8(2) . . . . ? Si1 N3 Si1 C14 79.27(15) 2 . . . ? Y1 N3 Si1 C14 -100.73(15) . . . . ? Si1 N3 Si1 C15 -162.14(12) 2 . . . ? Y1 N3 Si1 C15 17.86(12) . . . . ? Si1 N3 Si1 C16 -42.89(12) 2 . . . ? Y1 N3 Si1 C16 137.11(12) . . . . ? Si1 N3 Y1 N2 166.24(7) 2 . . . ? Si1 N3 Y1 N2 -13.76(7) . . . . ? Si1 N3 Y1 N2 -13.76(7) 2 . . 2 ? Si1 N3 Y1 N2 166.24(7) . . . 2 ? Si1 N3 Y1 N1 -122.39(6) 2 . . . ? Si1 N3 Y1 N1 57.61(6) . . . . ? Si1 N3 Y1 N1 57.61(6) 2 . . 2 ? Si1 N3 Y1 N1 -122.39(6) . . . 2 ? Si1 N3 Y1 Si1 180.0 . . . 2 ? C9 N2 Y1 N3 63.68(17) . . . . ? C10 N2 Y1 N3 -115.11(19) . . . . ? C9 N2 Y1 N2 -116.32(17) . . . 2 ? C10 N2 Y1 N2 64.89(19) . . . 2 ? C9 N2 Y1 N1 -16.69(15) . . . . ? C10 N2 Y1 N1 164.5(2) . . . . ? C9 N2 Y1 N1 169.28(16) . . . 2 ? C10 N2 Y1 N1 -9.5(2) . . . 2 ? C9 N2 Y1 Si1 78.5(2) . . . 2 ? C10 N2 Y1 Si1 -100.3(2) . . . 2 ? C5 N1 Y1 N3 42.5(3) . . . . ? C8 N1 Y1 N3 -114.28(14) . . . . ? C5 N1 Y1 N2 174.9(3) . . . . ? C8 N1 Y1 N2 18.16(14) . . . . ? C5 N1 Y1 N2 -91.4(3) . . . 2 ? C8 N1 Y1 N2 111.85(14) . . . 2 ? C5 N1 Y1 N1 -137.5(3) . . . 2 ? C8 N1 Y1 N1 65.72(14) . . . 2 ? C5 N1 Y1 Si1 19.8(3) . . . 2 ? C8 N1 Y1 Si1 -136.91(13) . . . 2 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.339 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.042 data_4b _database_code_depnum_ccdc_archive 'CCDC 896991' #TrackingRef 'CCDC 896991.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H60 Dy N5 Si2' _chemical_formula_weight 733.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.4062(18) _cell_length_b 16.8967(19) _cell_length_c 13.8325(16) _cell_angle_alpha 90.00 _cell_angle_beta 99.5270(10) _cell_angle_gamma 90.00 _cell_volume 3781.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9910 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.60 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 2.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5235 _exptl_absorpt_correction_T_max 0.7075 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14343 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3717 _reflns_number_gt 3475 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+2.7982P] 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 3717 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0221 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0511 _refine_ls_wR_factor_gt 0.0492 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0915(2) 0.2256(2) 0.0083(2) 0.0786(9) Uani 1 1 d . . . H1A H -0.0708 0.1851 0.0545 0.118 Uiso 1 1 calc R . . H1B H -0.1409 0.2073 -0.0326 0.118 Uiso 1 1 calc R . . H1C H -0.1038 0.2722 0.0429 0.118 Uiso 1 1 calc R . . C2 C -0.0087(3) 0.1702(2) -0.1113(3) 0.1114(16) Uani 1 1 d . . . H2A H 0.0346 0.1816 -0.1482 0.167 Uiso 1 1 calc R . . H2B H -0.0576 0.1544 -0.1552 0.167 Uiso 1 1 calc R . . H2C H 0.0086 0.1280 -0.0660 0.167 Uiso 1 1 calc R . . C3 C -0.0622(3) 0.3088(2) -0.1301(2) 0.0919(12) Uani 1 1 d . . . H3A H -0.0814 0.3532 -0.0968 0.138 Uiso 1 1 calc R . . H3B H -0.1073 0.2871 -0.1753 0.138 Uiso 1 1 calc R . . H3C H -0.0195 0.3258 -0.1651 0.138 Uiso 1 1 calc R . . C4 C -0.0274(2) 0.24490(17) -0.05421(18) 0.0679(8) Uani 1 1 d . . . C5 C 0.0504(2) 0.27629(16) 0.00593(19) 0.0587(7) Uani 1 1 d . . . C6 C 0.1259(3) 0.28908(19) -0.0264(3) 0.0800(10) Uani 1 1 d . . . H6 H 0.1389 0.2732 -0.0863 0.096 Uiso 1 1 calc R . . C7 C 0.1769(2) 0.3288(2) 0.0450(3) 0.0781(9) Uani 1 1 d . . . H7 H 0.2306 0.3454 0.0430 0.094 Uiso 1 1 calc R . . C8 C 0.13229(16) 0.33954(16) 0.1221(2) 0.0550(6) Uani 1 1 d . . . C9 C 0.15582(15) 0.38317(15) 0.2087(2) 0.0551(6) Uani 1 1 d . . . H9 H 0.2071 0.4081 0.2177 0.066 Uiso 1 1 calc R . . C10 C 0.13785(15) 0.45276(15) 0.35445(19) 0.0537(6) Uani 1 1 d . . . C11 C 0.1554(2) 0.53096(17) 0.3058(2) 0.0762(9) Uani 1 1 d . . . H11A H 0.2011 0.5240 0.2712 0.114 Uiso 1 1 calc R . . H11B H 0.1689 0.5710 0.3551 0.114 Uiso 1 1 calc R . . H11C H 0.1074 0.5469 0.2606 0.114 Uiso 1 1 calc R . . C12 C 0.2153(2) 0.4253(2) 0.4233(3) 0.0876(10) Uani 1 1 d . . . H12A H 0.2042 0.3760 0.4531 0.131 Uiso 1 1 calc R . . H12B H 0.2308 0.4643 0.4733 0.131 Uiso 1 1 calc R . . H12C H 0.2596 0.4182 0.3866 0.131 Uiso 1 1 calc R . . C13 C 0.06769(19) 0.46622(18) 0.4108(2) 0.0710(8) Uani 1 1 d . . . H13A H 0.0200 0.4846 0.3668 0.107 Uiso 1 1 calc R . . H13B H 0.0838 0.5051 0.4608 0.107 Uiso 1 1 calc R . . H13C H 0.0547 0.4175 0.4404 0.107 Uiso 1 1 calc R . . C14 C -0.1003(2) 0.0750(2) 0.3773(2) 0.0882(11) Uani 1 1 d . . . H14A H -0.0513 0.0459 0.4035 0.132 Uiso 1 1 calc R . . H14B H -0.1475 0.0409 0.3726 0.132 Uiso 1 1 calc R . . H14C H -0.1067 0.1187 0.4197 0.132 Uiso 1 1 calc R . . C15 C -0.18236(18) 0.17960(19) 0.2164(3) 0.0689(8) Uani 1 1 d . . . H15A H -0.1853 0.2171 0.2679 0.103 Uiso 1 1 calc R . . H15B H -0.2319 0.1484 0.2055 0.103 Uiso 1 1 calc R . . H15C H -0.1767 0.2073 0.1573 0.103 Uiso 1 1 calc R . . C16 C -0.1074(2) 0.02608(18) 0.1672(3) 0.0797(9) Uani 1 1 d . . . H16A H -0.1036 0.0431 0.1018 0.120 Uiso 1 1 calc R . . H16B H -0.1611 0.0039 0.1683 0.120 Uiso 1 1 calc R . . H16C H -0.0658 -0.0132 0.1878 0.120 Uiso 1 1 calc R . . Dy1 Dy 0.0000 0.295733(7) 0.2500 0.03593(6) Uani 1 2 d S . . N1 N 0.05476(14) 0.30607(11) 0.09833(15) 0.0473(5) Uani 1 1 d . . . N2 N 0.11087(11) 0.39119(11) 0.27736(14) 0.0461(4) Uani 1 1 d . . . N3 N 0.0000 0.16367(15) 0.2500 0.0411(5) Uani 1 2 d S . . Si1 Si -0.09087(4) 0.11318(4) 0.25270(5) 0.04977(15) Uani 1 1 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 C1 0.099(3) 0.075(2) 0.0576(16) -0.0032(15) -0.0010(16) -0.0179(18) C2 0.189(5) 0.077(2) 0.0625(19) -0.0236(18) 0.004(2) 0.033(3) C3 0.130(3) 0.087(2) 0.0583(17) 0.0172(16) 0.0137(19) 0.030(2) C4 0.110(2) 0.0528(16) 0.0418(12) -0.0029(11) 0.0143(14) 0.0141(16) C5 0.086(2) 0.0461(13) 0.0502(13) 0.0081(11) 0.0306(13) 0.0200(13) C6 0.104(3) 0.077(2) 0.072(2) 0.0057(16) 0.054(2) 0.0217(19) C7 0.072(2) 0.076(2) 0.099(2) 0.0202(19) 0.0533(19) 0.0177(17) C8 0.0523(14) 0.0483(14) 0.0706(15) 0.0125(12) 0.0285(12) 0.0108(11) C9 0.0396(12) 0.0478(14) 0.0796(16) 0.0140(12) 0.0152(11) 0.0019(10) C10 0.0468(13) 0.0459(13) 0.0650(14) 0.0033(11) -0.0010(11) -0.0128(11) C11 0.089(2) 0.0489(16) 0.089(2) 0.0039(15) 0.0117(17) -0.0201(15) C12 0.068(2) 0.087(2) 0.095(2) 0.0130(19) -0.0220(17) -0.0101(18) C13 0.0749(19) 0.0626(18) 0.0766(18) -0.0194(14) 0.0155(15) -0.0205(15) C14 0.086(2) 0.100(3) 0.077(2) 0.0169(18) 0.0094(17) -0.045(2) C15 0.0490(15) 0.0600(17) 0.099(2) -0.0072(16) 0.0162(15) -0.0076(13) C16 0.081(2) 0.0505(16) 0.102(2) -0.0234(16) -0.0018(18) -0.0107(15) Dy1 0.03520(8) 0.03108(8) 0.04309(8) 0.000 0.01115(5) 0.000 N1 0.0559(12) 0.0414(11) 0.0481(10) 0.0054(8) 0.0187(9) 0.0088(9) N2 0.0382(9) 0.0387(10) 0.0611(11) 0.0058(9) 0.0075(8) -0.0017(8) N3 0.0445(14) 0.0323(13) 0.0464(13) 0.000 0.0070(11) 0.000 Si1 0.0528(4) 0.0381(3) 0.0574(4) -0.0023(3) 0.0062(3) -0.0105(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 C1 C4 1.504(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C4 1.547(4) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.548(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.501(5) . ? C5 N1 1.365(3) . ? C5 C6 1.400(5) . ? C6 C7 1.360(6) . ? C6 H6 0.9300 . ? C7 C8 1.402(4) . ? C7 H7 0.9300 . ? C8 N1 1.381(3) . ? C8 C9 1.405(4) . ? C9 N2 1.302(3) . ? C9 H9 0.9300 . ? C10 N2 1.503(3) . ? C10 C13 1.510(4) . ? C10 C12 1.528(4) . ? C10 C11 1.532(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 Si1 1.870(3) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 Si1 1.875(3) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 Si1 1.880(3) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? Dy1 N3 2.232(3) . ? Dy1 N2 2.4136(19) . ? Dy1 N2 2.4136(19) 2 ? Dy1 N1 2.421(2) 2 ? Dy1 N1 2.421(2) . ? N3 Si1 1.7234(14) 2 ? N3 Si1 1.7234(14) . ? 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 C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C1 111.7(2) . . ? C5 C4 C2 110.4(3) . . ? C1 C4 C2 109.5(3) . . ? C5 C4 C3 108.3(3) . . ? C1 C4 C3 109.0(3) . . ? C2 C4 C3 107.8(3) . . ? N1 C5 C6 109.3(3) . . ? N1 C5 C4 123.9(2) . . ? C6 C5 C4 126.4(3) . . ? C7 C6 C5 108.4(3) . . ? C7 C6 H6 125.8 . . ? C5 C6 H6 125.8 . . ? C6 C7 C8 106.3(3) . . ? C6 C7 H7 126.9 . . ? C8 C7 H7 126.9 . . ? N1 C8 C7 110.0(3) . . ? N1 C8 C9 122.0(2) . . ? C7 C8 C9 127.8(3) . . ? N2 C9 C8 124.6(2) . . ? N2 C9 H9 117.7 . . ? C8 C9 H9 117.7 . . ? N2 C10 C13 108.1(2) . . ? N2 C10 C12 110.4(2) . . ? C13 C10 C12 110.5(3) . . ? N2 C10 C11 109.9(2) . . ? C13 C10 C11 108.2(3) . . ? C12 C10 C11 109.8(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 Dy1 N2 131.93(5) . . ? N3 Dy1 N2 131.93(5) . 2 ? N2 Dy1 N2 96.13(9) . 2 ? N3 Dy1 N1 94.14(4) . 2 ? N2 Dy1 N1 101.19(7) . 2 ? N2 Dy1 N1 73.12(7) 2 2 ? N3 Dy1 N1 94.14(4) . . ? N2 Dy1 N1 73.12(7) . . ? N2 Dy1 N1 101.19(7) 2 . ? N1 Dy1 N1 171.72(9) 2 . ? C5 N1 C8 106.1(2) . . ? C5 N1 Dy1 144.67(19) . . ? C8 N1 Dy1 106.40(15) . . ? C9 N2 C10 117.0(2) . . ? C9 N2 Dy1 108.62(16) . . ? C10 N2 Dy1 134.40(15) . . ? Si1 N3 Si1 120.67(15) 2 . ? Si1 N3 Dy1 119.67(8) 2 . ? Si1 N3 Dy1 119.67(8) . . ? N3 Si1 C14 113.21(11) . . ? N3 Si1 C15 110.80(12) . . ? C14 Si1 C15 105.58(17) . . ? N3 Si1 C16 114.13(13) . . ? C14 Si1 C16 106.55(17) . . ? C15 Si1 C16 105.96(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C4 C5 N1 -18.5(4) . . . . ? C2 C4 C5 N1 -140.6(3) . . . . ? C3 C4 C5 N1 101.6(3) . . . . ? C1 C4 C5 C6 170.1(3) . . . . ? C2 C4 C5 C6 48.0(4) . . . . ? C3 C4 C5 C6 -69.8(4) . . . . ? N1 C5 C6 C7 -1.5(4) . . . . ? C4 C5 C6 C7 170.9(3) . . . . ? C5 C6 C7 C8 0.6(4) . . . . ? C6 C7 C8 N1 0.5(3) . . . . ? C6 C7 C8 C9 -174.1(3) . . . . ? N1 C8 C9 N2 5.5(4) . . . . ? C7 C8 C9 N2 179.5(3) . . . . ? C6 C5 N1 C8 1.8(3) . . . . ? C4 C5 N1 C8 -170.9(2) . . . . ? C6 C5 N1 Dy1 -154.4(2) . . . . ? C4 C5 N1 Dy1 32.9(4) . . . . ? C7 C8 N1 C5 -1.4(3) . . . . ? C9 C8 N1 C5 173.5(2) . . . . ? C7 C8 N1 Dy1 164.51(19) . . . . ? C9 C8 N1 Dy1 -20.6(3) . . . . ? N3 Dy1 N1 C5 42.2(3) . . . . ? N2 Dy1 N1 C5 174.9(3) . . . . ? N2 Dy1 N1 C5 -92.1(3) 2 . . . ? N1 Dy1 N1 C5 -137.8(3) 2 . . . ? N3 Dy1 N1 C8 -113.99(14) . . . . ? N2 Dy1 N1 C8 18.71(14) . . . . ? N2 Dy1 N1 C8 111.80(15) 2 . . . ? N1 Dy1 N1 C8 66.01(14) 2 . . . ? C8 C9 N2 C10 -168.0(2) . . . . ? C8 C9 N2 Dy1 13.5(3) . . . . ? C13 C10 N2 C9 166.3(2) . . . . ? C12 C10 N2 C9 -72.7(3) . . . . ? C11 C10 N2 C9 48.5(3) . . . . ? C13 C10 N2 Dy1 -15.6(3) . . . . ? C12 C10 N2 Dy1 105.4(3) . . . . ? C11 C10 N2 Dy1 -133.4(2) . . . . ? N3 Dy1 N2 C9 63.24(17) . . . . ? N2 Dy1 N2 C9 -116.76(17) 2 . . . ? N1 Dy1 N2 C9 169.29(16) 2 . . . ? N1 Dy1 N2 C9 -16.90(15) . . . . ? N3 Dy1 N2 C10 -115.00(19) . . . . ? N2 Dy1 N2 C10 65.00(19) 2 . . . ? N1 Dy1 N2 C10 -8.9(2) 2 . . . ? N1 Dy1 N2 C10 164.9(2) . . . . ? N2 Dy1 N3 Si1 -13.41(7) . . . 2 ? N2 Dy1 N3 Si1 166.59(7) 2 . . 2 ? N1 Dy1 N3 Si1 -122.46(6) 2 . . 2 ? N1 Dy1 N3 Si1 57.54(6) . . . 2 ? N2 Dy1 N3 Si1 166.59(7) . . . . ? N2 Dy1 N3 Si1 -13.41(7) 2 . . . ? N1 Dy1 N3 Si1 57.54(6) 2 . . . ? N1 Dy1 N3 Si1 -122.46(6) . . . . ? Si1 N3 Si1 C14 79.20(16) 2 . . . ? Dy1 N3 Si1 C14 -100.80(16) . . . . ? Si1 N3 Si1 C15 -162.41(12) 2 . . . ? Dy1 N3 Si1 C15 17.59(12) . . . . ? Si1 N3 Si1 C16 -42.92(13) 2 . . . ? Dy1 N3 Si1 C16 137.08(13) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.557 _refine_diff_density_min -0.802 _refine_diff_density_rms 0.058 data_4c _database_code_depnum_ccdc_archive 'CCDC 896992' #TrackingRef 'CCDC 896992.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H60 Er N5 Si2' _chemical_formula_weight 738.29 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.3623(12) _cell_length_b 16.8981(13) _cell_length_c 13.8066(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.0760(10) _cell_angle_gamma 90.00 _cell_volume 3769.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7632 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 26.93 _exptl_crystal_description block _exptl_crystal_colour reddish _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1532 _exptl_absorpt_coefficient_mu 2.316 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5736 _exptl_absorpt_correction_T_max 0.7083 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14472 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3703 _reflns_number_gt 3255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+2.4975P] 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 3703 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0583 _refine_ls_wR_factor_gt 0.0549 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Er1 Er 0.5000 0.296631(11) 0.2500 0.03891(7) Uani 1 2 d S . . Si1 Si 0.40924(6) 0.11431(5) 0.25358(7) 0.0535(2) Uani 1 1 d . . . N1 N 0.44617(17) 0.30573(14) 0.4011(2) 0.0502(6) Uani 1 1 d . . . N2 N 0.38948(15) 0.38987(15) 0.22227(19) 0.0479(6) Uani 1 1 d . . . N3 N 0.5000 0.1651(2) 0.2500 0.0461(8) Uani 1 2 d S . . C1 C 0.5929(3) 0.2259(3) 0.4906(3) 0.0827(13) Uani 1 1 d . . . H1A H 0.5727 0.1849 0.4450 0.124 Uiso 1 1 calc R . . H1B H 0.6425 0.2083 0.5315 0.124 Uiso 1 1 calc R . . H1C H 0.6046 0.2724 0.4553 0.124 Uiso 1 1 calc R . . C2 C 0.5092(4) 0.1697(3) 0.6112(3) 0.113(2) Uani 1 1 d . . . H2A H 0.4898 0.1283 0.5658 0.170 Uiso 1 1 calc R . . H2B H 0.4675 0.1818 0.6506 0.170 Uiso 1 1 calc R . . H2C H 0.5587 0.1527 0.6528 0.170 Uiso 1 1 calc R . . C3 C 0.5621(3) 0.3087(3) 0.6299(3) 0.0944(15) Uani 1 1 d . . . H3A H 0.6084 0.2877 0.6738 0.142 Uiso 1 1 calc R . . H3B H 0.5194 0.3239 0.6666 0.142 Uiso 1 1 calc R . . H3C H 0.5795 0.3541 0.5967 0.142 Uiso 1 1 calc R . . C4 C 0.5282(3) 0.2448(2) 0.5536(3) 0.0716(11) Uani 1 1 d . . . C5 C 0.4503(3) 0.27640(19) 0.4937(3) 0.0606(10) Uani 1 1 d . . . C6 C 0.3748(3) 0.2892(2) 0.5269(3) 0.0828(14) Uani 1 1 d . . . H6 H 0.3621 0.2735 0.5873 0.099 Uiso 1 1 calc R . . C7 C 0.3232(3) 0.3284(3) 0.4561(4) 0.0797(12) Uani 1 1 d . . . H7 H 0.2693 0.3446 0.4587 0.096 Uiso 1 1 calc R . . C8 C 0.3679(2) 0.3393(2) 0.3783(3) 0.0576(9) Uani 1 1 d . . . C9 C 0.34431(19) 0.38217(19) 0.2922(3) 0.0558(8) Uani 1 1 d . . . H9 H 0.2930 0.4071 0.2837 0.067 Uiso 1 1 calc R . . C10 C 0.3626(2) 0.45188(19) 0.1450(3) 0.0548(8) Uani 1 1 d . . . C11 C 0.3453(3) 0.5301(2) 0.1954(3) 0.0772(12) Uani 1 1 d . . . H11A H 0.3933 0.5450 0.2412 0.116 Uiso 1 1 calc R . . H11B H 0.2991 0.5233 0.2295 0.116 Uiso 1 1 calc R . . H11C H 0.3330 0.5708 0.1468 0.116 Uiso 1 1 calc R . . C12 C 0.2850(3) 0.4249(3) 0.0771(3) 0.0897(14) Uani 1 1 d . . . H12A H 0.2701 0.4637 0.0266 0.135 Uiso 1 1 calc R . . H12B H 0.2405 0.4188 0.1142 0.135 Uiso 1 1 calc R . . H12C H 0.2956 0.3752 0.0478 0.135 Uiso 1 1 calc R . . C13 C 0.4331(2) 0.4659(2) 0.0891(3) 0.0736(11) Uani 1 1 d . . . H13A H 0.4809 0.4832 0.1335 0.110 Uiso 1 1 calc R . . H13B H 0.4177 0.5058 0.0401 0.110 Uiso 1 1 calc R . . H13C H 0.4458 0.4176 0.0579 0.110 Uiso 1 1 calc R . . C15 C 0.3172(2) 0.1797(2) 0.2173(3) 0.0723(11) Uani 1 1 d . . . H15A H 0.3067 0.2095 0.2733 0.108 Uiso 1 1 calc R . . H15B H 0.2697 0.1478 0.1935 0.108 Uiso 1 1 calc R . . H15C H 0.3278 0.2153 0.1666 0.108 Uiso 1 1 calc R . . C14 C 0.4000(3) 0.0759(3) 0.3782(3) 0.0932(15) Uani 1 1 d . . . H14A H 0.4482 0.0453 0.4029 0.140 Uiso 1 1 calc R . . H14B H 0.3516 0.0433 0.3742 0.140 Uiso 1 1 calc R . . H14C H 0.3954 0.1196 0.4216 0.140 Uiso 1 1 calc R . . C16 C 0.3935(3) 0.0270(2) 0.1680(3) 0.0826(13) Uani 1 1 d . . . H16A H 0.4001 0.0435 0.1032 0.124 Uiso 1 1 calc R . . H16B H 0.3388 0.0061 0.1668 0.124 Uiso 1 1 calc R . . H16C H 0.4335 -0.0132 0.1904 0.124 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.03985(10) 0.03171(10) 0.04712(12) 0.000 0.01286(8) 0.000 Si1 0.0594(5) 0.0387(5) 0.0621(6) -0.0024(4) 0.0086(4) -0.0110(4) N1 0.0601(16) 0.0412(15) 0.0531(16) -0.0044(12) 0.0210(13) -0.0084(12) N2 0.0443(13) 0.0385(14) 0.0612(17) -0.0075(12) 0.0093(12) 0.0002(11) N3 0.055(2) 0.0291(18) 0.055(2) 0.000 0.0098(17) 0.000 C1 0.102(3) 0.082(3) 0.059(3) 0.002(2) -0.001(2) 0.021(2) C2 0.190(6) 0.078(3) 0.067(3) 0.024(3) 0.004(3) -0.034(4) C3 0.134(4) 0.088(3) 0.061(3) -0.017(2) 0.016(3) -0.028(3) C4 0.113(3) 0.057(2) 0.045(2) 0.0020(17) 0.012(2) -0.014(2) C5 0.091(3) 0.0451(19) 0.053(2) -0.0072(15) 0.032(2) -0.0189(17) C6 0.114(4) 0.077(3) 0.071(3) -0.006(2) 0.057(3) -0.024(3) C7 0.075(3) 0.077(3) 0.099(3) -0.020(3) 0.051(3) -0.018(2) C8 0.060(2) 0.0460(19) 0.073(2) -0.0126(17) 0.0296(18) -0.0104(16) C9 0.0431(16) 0.0443(18) 0.082(3) -0.0134(18) 0.0159(17) 0.0014(14) C10 0.0485(17) 0.0453(18) 0.068(2) -0.0040(16) -0.0001(16) 0.0093(14) C11 0.095(3) 0.049(2) 0.087(3) -0.003(2) 0.014(2) 0.022(2) C12 0.076(3) 0.090(3) 0.093(3) -0.009(3) -0.019(2) 0.012(2) C13 0.079(3) 0.064(2) 0.080(3) 0.020(2) 0.020(2) 0.022(2) C15 0.057(2) 0.057(2) 0.105(3) -0.007(2) 0.019(2) -0.0103(17) C14 0.090(3) 0.102(3) 0.087(3) 0.016(3) 0.014(2) -0.046(3) C16 0.087(3) 0.053(2) 0.103(3) -0.022(2) 0.001(2) -0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 N3 2.223(3) . ? Er1 N2 2.383(2) 2_655 ? Er1 N2 2.383(2) . ? Er1 N1 2.393(3) . ? Er1 N1 2.393(3) 2_655 ? Si1 N3 1.7226(19) . ? Si1 C14 1.867(4) . ? Si1 C15 1.872(4) . ? Si1 C16 1.882(4) . ? N1 C5 1.364(4) . ? N1 C8 1.390(4) . ? N2 C9 1.311(4) . ? N2 C10 1.511(4) . ? N3 Si1 1.7226(19) 2_655 ? C1 C4 1.505(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C4 1.556(6) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.549(5) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.504(6) . ? C5 C6 1.399(6) . ? C6 C7 1.358(7) . ? C6 H6 0.9300 . ? C7 C8 1.404(5) . ? C7 H7 0.9300 . ? C8 C9 1.394(5) . ? C9 H9 0.9300 . ? C10 C13 1.505(5) . ? C10 C12 1.523(5) . ? C10 C11 1.540(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Er1 N2 131.38(6) . 2_655 ? N3 Er1 N2 131.38(6) . . ? N2 Er1 N2 97.24(12) 2_655 . ? N3 Er1 N1 93.68(6) . . ? N2 Er1 N1 101.05(9) 2_655 . ? N2 Er1 N1 73.94(9) . . ? N3 Er1 N1 93.68(6) . 2_655 ? N2 Er1 N1 73.94(9) 2_655 2_655 ? N2 Er1 N1 101.05(9) . 2_655 ? N1 Er1 N1 172.63(12) . 2_655 ? N3 Si1 C14 113.28(14) . . ? N3 Si1 C15 111.07(15) . . ? C14 Si1 C15 105.8(2) . . ? N3 Si1 C16 113.94(16) . . ? C14 Si1 C16 106.5(2) . . ? C15 Si1 C16 105.66(19) . . ? C5 N1 C8 105.5(3) . . ? C5 N1 Er1 145.5(2) . . ? C8 N1 Er1 106.3(2) . . ? C9 N2 C10 117.0(3) . . ? C9 N2 Er1 108.5(2) . . ? C10 N2 Er1 134.5(2) . . ? Si1 N3 Si1 120.2(2) . 2_655 ? Si1 N3 Er1 119.88(10) . . ? Si1 N3 Er1 119.88(10) 2_655 . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C1 111.8(3) . . ? C5 C4 C3 108.0(4) . . ? C1 C4 C3 109.4(4) . . ? C5 C4 C2 110.5(4) . . ? C1 C4 C2 109.7(4) . . ? C3 C4 C2 107.4(3) . . ? N1 C5 C6 109.6(4) . . ? N1 C5 C4 123.8(3) . . ? C6 C5 C4 126.2(4) . . ? C7 C6 C5 108.7(4) . . ? C7 C6 H6 125.7 . . ? C5 C6 H6 125.7 . . ? C6 C7 C8 106.0(4) . . ? C6 C7 H7 127.0 . . ? C8 C7 H7 127.0 . . ? N1 C8 C9 121.8(3) . . ? N1 C8 C7 110.2(4) . . ? C9 C8 C7 127.8(4) . . ? N2 C9 C8 124.5(3) . . ? N2 C9 H9 117.7 . . ? C8 C9 H9 117.7 . . ? N2 C10 C13 108.0(3) . . ? N2 C10 C12 110.4(3) . . ? C13 C10 C12 111.3(3) . . ? N2 C10 C11 109.3(3) . . ? C13 C10 C11 107.9(3) . . ? C12 C10 C11 109.9(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Er1 N1 C5 42.6(4) . . . . ? N2 Er1 N1 C5 -90.8(4) 2_655 . . . ? N2 Er1 N1 C5 174.7(4) . . . . ? N1 Er1 N1 C5 -137.4(4) 2_655 . . . ? N3 Er1 N1 C8 -114.00(19) . . . . ? N2 Er1 N1 C8 112.56(19) 2_655 . . . ? N2 Er1 N1 C8 18.12(19) . . . . ? N1 Er1 N1 C8 66.00(19) 2_655 . . . ? N3 Er1 N2 C9 64.2(2) . . . . ? N2 Er1 N2 C9 -115.8(2) 2_655 . . . ? N1 Er1 N2 C9 -16.3(2) . . . . ? N1 Er1 N2 C9 169.3(2) 2_655 . . . ? N3 Er1 N2 C10 -115.5(2) . . . . ? N2 Er1 N2 C10 64.5(2) 2_655 . . . ? N1 Er1 N2 C10 164.0(3) . . . . ? N1 Er1 N2 C10 -10.4(3) 2_655 . . . ? C14 Si1 N3 Si1 79.11(19) . . . 2_655 ? C15 Si1 N3 Si1 -161.97(16) . . . 2_655 ? C16 Si1 N3 Si1 -42.78(16) . . . 2_655 ? C14 Si1 N3 Er1 -100.89(19) . . . . ? C15 Si1 N3 Er1 18.03(16) . . . . ? C16 Si1 N3 Er1 137.22(16) . . . . ? N2 Er1 N3 Si1 165.92(9) 2_655 . . . ? N2 Er1 N3 Si1 -14.08(9) . . . . ? N1 Er1 N3 Si1 57.70(8) . . . . ? N1 Er1 N3 Si1 -122.30(8) 2_655 . . . ? N2 Er1 N3 Si1 -14.08(9) 2_655 . . 2_655 ? N2 Er1 N3 Si1 165.92(9) . . . 2_655 ? N1 Er1 N3 Si1 -122.30(8) . . . 2_655 ? N1 Er1 N3 Si1 57.70(8) 2_655 . . 2_655 ? C8 N1 C5 C6 1.9(4) . . . . ? Er1 N1 C5 C6 -154.8(3) . . . . ? C8 N1 C5 C4 -171.1(3) . . . . ? Er1 N1 C5 C4 32.2(6) . . . . ? C1 C4 C5 N1 -17.7(5) . . . . ? C3 C4 C5 N1 102.7(4) . . . . ? C2 C4 C5 N1 -140.2(4) . . . . ? C1 C4 C5 C6 170.4(4) . . . . ? C3 C4 C5 C6 -69.2(5) . . . . ? C2 C4 C5 C6 48.0(5) . . . . ? N1 C5 C6 C7 -1.4(5) . . . . ? C4 C5 C6 C7 171.4(4) . . . . ? C5 C6 C7 C8 0.3(5) . . . . ? C5 N1 C8 C9 173.6(3) . . . . ? Er1 N1 C8 C9 -19.9(4) . . . . ? C5 N1 C8 C7 -1.7(4) . . . . ? Er1 N1 C8 C7 164.8(2) . . . . ? C6 C7 C8 N1 0.9(4) . . . . ? C6 C7 C8 C9 -174.1(4) . . . . ? C10 N2 C9 C8 -167.5(3) . . . . ? Er1 N2 C9 C8 12.8(4) . . . . ? N1 C8 C9 N2 5.5(5) . . . . ? C7 C8 C9 N2 180.0(4) . . . . ? C9 N2 C10 C13 165.2(3) . . . . ? Er1 N2 C10 C13 -15.1(4) . . . . ? C9 N2 C10 C12 -72.8(4) . . . . ? Er1 N2 C10 C12 106.9(3) . . . . ? C9 N2 C10 C11 48.2(4) . . . . ? Er1 N2 C10 C11 -132.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.747 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.064 data_5 _database_code_depnum_ccdc_archive 'CCDC 896993' #TrackingRef 'CCDC 896993.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H66 Li4 N6 Si4' _chemical_formula_weight 651.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 10.8200(9) _cell_length_b 13.6124(12) _cell_length_c 14.8062(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.2780(10) _cell_angle_gamma 90.00 _cell_volume 2180.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4371 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 23.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.161 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9549 _exptl_absorpt_correction_T_max 0.9732 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18610 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4990 _reflns_number_gt 2820 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+0.3954P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4990 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1044 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1537 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5734(2) 0.49303(18) 0.13217(16) 0.0670(6) Uani 1 1 d . . . H1 H 0.5199 0.4544 0.1660 0.080 Uiso 1 1 calc R . . C2 C 0.6973(3) 0.47635(19) 0.12473(17) 0.0711(7) Uani 1 1 d . . . H2 H 0.7421 0.4256 0.1513 0.085 Uiso 1 1 calc R . . C3 C 0.7434(2) 0.55073(18) 0.06909(17) 0.0644(6) Uani 1 1 d . . . H3 H 0.8251 0.5591 0.0514 0.077 Uiso 1 1 calc R . . C4 C 0.64473(19) 0.60885(15) 0.04570(14) 0.0519(5) Uani 1 1 d . . . C5 C 0.6413(2) 0.70216(16) -0.00647(16) 0.0621(6) Uani 1 1 d . . . H5A H 0.7251 0.7223 -0.0204 0.074 Uiso 1 1 calc R . . H5B H 0.5980 0.6914 -0.0631 0.074 Uiso 1 1 calc R . . C6 C 0.6561(2) 0.84516(17) 0.10338(18) 0.0652(6) Uani 1 1 d . . . C7 C 0.7160(4) 0.7834(3) 0.1761(3) 0.1321(15) Uani 1 1 d . . . H7A H 0.6531 0.7536 0.2126 0.198 Uiso 1 1 calc R . . H7B H 0.7676 0.8242 0.2134 0.198 Uiso 1 1 calc R . . H7C H 0.7653 0.7330 0.1487 0.198 Uiso 1 1 calc R . . C8 C 0.7557(3) 0.8980(3) 0.0503(3) 0.1306(15) Uani 1 1 d . . . H8A H 0.8145 0.8510 0.0283 0.196 Uiso 1 1 calc R . . H8B H 0.7969 0.9445 0.0888 0.196 Uiso 1 1 calc R . . H8C H 0.7186 0.9319 0.0001 0.196 Uiso 1 1 calc R . . C9 C 0.5722(3) 0.9211(2) 0.1449(3) 0.1126(12) Uani 1 1 d . . . H9A H 0.5285 0.9554 0.0979 0.169 Uiso 1 1 calc R . . H9B H 0.6206 0.9670 0.1793 0.169 Uiso 1 1 calc R . . H9C H 0.5139 0.8893 0.1839 0.169 Uiso 1 1 calc R . . C10 C 0.0747(3) 0.6747(3) 0.2379(3) 0.1291(14) Uani 1 1 d . . . H10A H 0.0810 0.7444 0.2472 0.194 Uiso 1 1 calc R . . H10B H 0.0588 0.6429 0.2945 0.194 Uiso 1 1 calc R . . H10C H 0.0083 0.6612 0.1965 0.194 Uiso 1 1 calc R . . C11 C 0.2064(3) 0.4900(2) 0.18355(19) 0.0988(10) Uani 1 1 d . . . H11A H 0.1391 0.4737 0.1438 0.148 Uiso 1 1 calc R . . H11B H 0.1900 0.4644 0.2427 0.148 Uiso 1 1 calc R . . H11C H 0.2814 0.4617 0.1609 0.148 Uiso 1 1 calc R . . C12 C 0.3446(3) 0.6510(3) 0.27870(19) 0.1056(11) Uani 1 1 d . . . H12A H 0.4216 0.6228 0.2600 0.158 Uiso 1 1 calc R . . H12B H 0.3194 0.6218 0.3347 0.158 Uiso 1 1 calc R . . H12C H 0.3546 0.7205 0.2868 0.158 Uiso 1 1 calc R . . C13 C 0.0484(2) 0.6943(2) -0.0285(2) 0.0970(10) Uani 1 1 d . . . H13A H 0.0731 0.6404 -0.0661 0.145 Uiso 1 1 calc R . . H13B H 0.0047 0.7419 -0.0642 0.145 Uiso 1 1 calc R . . H13C H -0.0046 0.6707 0.0186 0.145 Uiso 1 1 calc R . . C14 C 0.2874(3) 0.7976(2) -0.07305(19) 0.0798(8) Uani 1 1 d . . . H14A H 0.3479 0.8431 -0.0505 0.120 Uiso 1 1 calc R . . H14B H 0.2361 0.8297 -0.1171 0.120 Uiso 1 1 calc R . . H14C H 0.3284 0.7427 -0.1005 0.120 Uiso 1 1 calc R . . C15 C 0.1346(3) 0.8678(2) 0.0803(2) 0.1063(11) Uani 1 1 d . . . H15A H 0.0761 0.8511 0.1264 0.159 Uiso 1 1 calc R . . H15B H 0.0959 0.9102 0.0368 0.159 Uiso 1 1 calc R . . H15C H 0.2039 0.9010 0.1072 0.159 Uiso 1 1 calc R . . Li1 Li 0.4463(3) 0.7026(3) 0.1123(3) 0.0662(10) Uani 1 1 d . . . Li2 Li 0.3587(3) 0.5630(3) 0.0232(3) 0.0613(10) Uani 1 1 d . . . N1 N 0.53768(16) 0.57400(13) 0.08354(12) 0.0571(5) Uani 1 1 d . . . N2 N 0.57887(16) 0.78162(13) 0.04459(13) 0.0597(5) Uani 1 1 d . . . H2A H 0.5396 0.8210 0.0039 0.072 Uiso 1 1 calc R . . N3 N 0.27070(15) 0.67562(13) 0.09066(12) 0.0558(5) Uani 1 1 d . . . Si1 Si 0.22343(6) 0.62745(6) 0.18987(5) 0.0694(2) Uani 1 1 d . . . Si2 Si 0.18900(6) 0.75293(5) 0.02302(5) 0.0639(2) Uani 1 1 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 C1 0.0878(18) 0.0554(15) 0.0577(14) 0.0074(12) 0.0029(13) -0.0088(13) C2 0.0863(18) 0.0636(16) 0.0631(16) 0.0013(13) -0.0193(13) 0.0087(13) C3 0.0594(13) 0.0627(15) 0.0712(16) -0.0106(13) -0.0059(12) -0.0002(11) C4 0.0590(12) 0.0470(12) 0.0496(12) -0.0077(10) 0.0003(10) -0.0065(10) C5 0.0763(15) 0.0503(13) 0.0596(14) -0.0041(11) 0.0064(11) -0.0096(11) C6 0.0651(14) 0.0518(14) 0.0787(17) -0.0154(12) 0.0048(12) -0.0064(11) C7 0.190(4) 0.096(3) 0.109(3) -0.034(2) -0.071(3) 0.016(3) C8 0.112(3) 0.109(3) 0.171(4) -0.051(3) 0.051(3) -0.055(2) C9 0.106(2) 0.085(2) 0.147(3) -0.042(2) 0.021(2) 0.0120(18) C10 0.108(3) 0.161(4) 0.119(3) 0.008(3) 0.063(2) 0.013(2) C11 0.128(3) 0.088(2) 0.0806(19) 0.0104(17) 0.0218(18) -0.0339(19) C12 0.125(3) 0.133(3) 0.0584(17) -0.0018(18) 0.0024(17) -0.030(2) C13 0.0658(17) 0.105(2) 0.120(3) 0.001(2) -0.0204(17) -0.0061(16) C14 0.0860(18) 0.0737(18) 0.0796(18) 0.0188(15) -0.0076(14) -0.0041(14) C15 0.115(2) 0.077(2) 0.127(3) -0.0101(19) 0.010(2) 0.0171(18) Li1 0.058(2) 0.063(2) 0.078(3) -0.012(2) 0.0064(19) -0.0083(18) Li2 0.064(2) 0.059(2) 0.060(2) -0.0032(19) -0.0050(18) -0.0075(18) N1 0.0621(11) 0.0528(11) 0.0566(11) 0.0021(9) 0.0022(9) -0.0049(9) N2 0.0595(11) 0.0468(10) 0.0730(13) 0.0005(9) -0.0011(9) -0.0014(8) N3 0.0508(10) 0.0600(11) 0.0566(11) -0.0004(9) 0.0049(8) -0.0073(8) Si1 0.0706(4) 0.0793(5) 0.0584(4) -0.0027(4) 0.0177(3) -0.0147(4) Si2 0.0560(4) 0.0590(4) 0.0766(5) -0.0011(4) -0.0015(3) -0.0019(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 C1 C2 1.365(3) . ? C1 N1 1.371(3) . ? C1 Li2 2.536(5) 3_665 ? C2 C3 1.399(3) . ? C2 Li2 2.332(4) 3_665 ? C3 C4 1.372(3) . ? C3 Li2 2.339(4) 3_665 ? C4 N1 1.374(3) . ? C4 C5 1.487(3) . ? C4 Li2 2.553(4) 3_665 ? C5 N2 1.484(3) . ? C6 N2 1.482(3) . ? C6 C9 1.509(3) . ? C6 C7 1.510(4) . ? C6 C8 1.518(4) . ? C10 Si1 1.876(3) . ? C11 Si1 1.883(3) . ? C12 Si1 1.880(3) . ? C13 Si2 1.876(3) . ? C14 Si2 1.882(3) . ? C15 Si2 1.876(3) . ? Li1 N3 1.960(4) . ? Li1 N1 2.057(4) . ? Li1 N2 2.057(4) . ? Li2 N3 2.064(4) . ? Li2 N1 2.134(4) . ? Li2 C2 2.332(4) 3_665 ? Li2 C3 2.339(4) 3_665 ? Li2 C1 2.536(5) 3_665 ? Li2 C4 2.553(4) 3_665 ? Li2 N1 2.693(4) 3_665 ? N1 Li2 2.693(4) 3_665 ? N3 Si1 1.6902(19) . ? N3 Si2 1.698(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 111.5(2) . . ? C2 C1 Li2 65.64(16) . 3_665 ? N1 C1 Li2 81.24(15) . 3_665 ? C1 C2 C3 106.3(2) . . ? C1 C2 Li2 82.15(18) . 3_665 ? C3 C2 Li2 72.85(16) . 3_665 ? C4 C3 C2 106.7(2) . . ? C4 C3 Li2 82.51(16) . 3_665 ? C2 C3 Li2 72.31(16) . 3_665 ? C3 C4 N1 110.8(2) . . ? C3 C4 C5 129.9(2) . . ? N1 C4 C5 119.22(19) . . ? C3 C4 Li2 65.29(15) . 3_665 ? N1 C4 Li2 80.56(14) . 3_665 ? C5 C4 Li2 125.10(17) . 3_665 ? N2 C5 C4 111.59(18) . . ? N2 C6 C9 107.4(2) . . ? N2 C6 C7 109.4(2) . . ? C9 C6 C7 110.4(3) . . ? N2 C6 C8 111.8(2) . . ? C9 C6 C8 108.4(2) . . ? C7 C6 C8 109.3(3) . . ? N3 Li1 N1 105.85(19) . . ? N3 Li1 N2 134.1(2) . . ? N1 Li1 N2 90.40(17) . . ? N3 Li2 N1 99.52(17) . . ? N3 Li2 C2 120.46(19) . 3_665 ? N1 Li2 C2 129.8(2) . 3_665 ? N3 Li2 C3 123.82(19) . 3_665 ? N1 Li2 C3 135.7(2) . 3_665 ? C2 Li2 C3 34.85(10) 3_665 3_665 ? N3 Li2 C1 143.0(2) . 3_665 ? N1 Li2 C1 97.70(16) . 3_665 ? C2 Li2 C1 32.21(9) 3_665 3_665 ? C3 Li2 C1 53.77(12) 3_665 3_665 ? N3 Li2 C4 150.23(19) . 3_665 ? N1 Li2 C4 104.04(17) . 3_665 ? C2 Li2 C4 53.89(12) 3_665 3_665 ? C3 Li2 C4 32.20(9) 3_665 3_665 ? C1 Li2 C4 50.60(10) 3_665 3_665 ? N3 Li2 N1 173.0(2) . 3_665 ? N1 Li2 N1 85.08(14) . 3_665 ? C2 Li2 N1 52.88(11) 3_665 3_665 ? C3 Li2 N1 52.79(11) 3_665 3_665 ? C1 Li2 N1 30.21(8) 3_665 3_665 ? C4 Li2 N1 30.21(7) 3_665 3_665 ? C1 N1 C4 104.82(19) . . ? C1 N1 Li1 135.27(19) . . ? C4 N1 Li1 101.40(17) . . ? C1 N1 Li2 114.61(18) . . ? C4 N1 Li2 128.23(18) . . ? Li1 N1 Li2 73.12(16) . . ? C1 N1 Li2 68.55(15) . 3_665 ? C4 N1 Li2 69.24(14) . 3_665 ? Li1 N1 Li2 155.95(17) . 3_665 ? Li2 N1 Li2 94.92(14) . 3_665 ? C6 N2 C5 117.85(18) . . ? C6 N2 Li1 114.30(18) . . ? C5 N2 Li1 100.82(17) . . ? Si1 N3 Si2 126.45(11) . . ? Si1 N3 Li1 103.18(16) . . ? Si2 N3 Li1 118.78(16) . . ? Si1 N3 Li2 105.94(14) . . ? Si2 N3 Li2 114.50(14) . . ? Li1 N3 Li2 76.67(16) . . ? N3 Si1 C10 117.38(15) . . ? N3 Si1 C12 109.20(12) . . ? C10 Si1 C12 105.83(18) . . ? N3 Si1 C11 111.86(11) . . ? C10 Si1 C11 106.02(17) . . ? C12 Si1 C11 105.79(16) . . ? N3 Si2 C13 113.26(12) . . ? N3 Si2 C15 114.42(13) . . ? C13 Si2 C15 106.42(15) . . ? N3 Si2 C14 110.55(11) . . ? C13 Si2 C14 106.91(14) . . ? C15 Si2 C14 104.65(14) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.224 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.036 data_7a _database_code_depnum_ccdc_archive 'CCDC 896994' #TrackingRef 'CCDC 896994.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H80 N6 Nd2 Si4' _chemical_formula_weight 1118.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.619(5) _cell_length_b 12.344(3) _cell_length_c 17.358(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.536(2) _cell_angle_gamma 90.00 _cell_volume 5545(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9951 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.51 _exptl_crystal_description block _exptl_crystal_colour bluish _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 1.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6598 _exptl_absorpt_correction_T_max 0.7304 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19673 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5423 _reflns_number_gt 4127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+34.4879P] 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 5423 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1167 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0340(2) 0.4629(6) 0.1204(3) 0.0565(16) Uani 1 1 d . . . H1 H -0.0241 0.3942 0.1404 0.068 Uiso 1 1 calc R . . C2 C -0.0814(3) 0.5094(7) 0.1167(4) 0.070(2) Uani 1 1 d . . . H2 H -0.1090 0.4780 0.1328 0.084 Uiso 1 1 calc R . . C3 C -0.0803(2) 0.6128(6) 0.0842(4) 0.0633(18) Uani 1 1 d . . . H3 H -0.1070 0.6632 0.0737 0.076 Uiso 1 1 calc R . . C4 C -0.0314(2) 0.6251(5) 0.0707(4) 0.0502(14) Uani 1 1 d . . . C5 C -0.0069(2) 0.7263(5) 0.0481(5) 0.0627(17) Uani 1 1 d . . . H5A H -0.0262 0.7505 -0.0035 0.075 Uiso 1 1 calc R . . H5B H -0.0087 0.7829 0.0862 0.075 Uiso 1 1 calc R . . C6 C 0.0756(2) 0.8081(4) 0.0552(3) 0.0439(12) Uani 1 1 d . . . C7 C 0.0761(2) 0.8746(5) -0.0102(4) 0.0531(14) Uani 1 1 d . . . C8 C 0.1078(3) 0.9647(6) 0.0001(5) 0.077(2) Uani 1 1 d . . . H8 H 0.1089 1.0080 -0.0433 0.092 Uiso 1 1 calc R . . C9 C 0.1372(4) 0.9911(7) 0.0727(6) 0.089(3) Uani 1 1 d . . . H9 H 0.1588 1.0514 0.0784 0.107 Uiso 1 1 calc R . . C10 C 0.1354(3) 0.9301(6) 0.1370(5) 0.078(2) Uani 1 1 d . . . H10 H 0.1550 0.9504 0.1866 0.093 Uiso 1 1 calc R . . C11 C 0.1046(2) 0.8377(5) 0.1302(4) 0.0543(15) Uani 1 1 d . . . C12 C 0.0430(3) 0.8494(6) -0.0914(4) 0.0656(18) Uani 1 1 d . . . H12 H 0.0244 0.7819 -0.0871 0.079 Uiso 1 1 calc R . . C13 C 0.0023(4) 0.9378(7) -0.1199(5) 0.093(3) Uani 1 1 d . . . H13A H 0.0193 1.0052 -0.1246 0.140 Uiso 1 1 calc R . . H13B H -0.0188 0.9455 -0.0823 0.140 Uiso 1 1 calc R . . H13C H -0.0190 0.9178 -0.1705 0.140 Uiso 1 1 calc R . . C14 C 0.0747(4) 0.8313(8) -0.1527(5) 0.096(3) Uani 1 1 d . . . H14A H 0.0998 0.7754 -0.1345 0.145 Uiso 1 1 calc R . . H14B H 0.0921 0.8972 -0.1601 0.145 Uiso 1 1 calc R . . H14C H 0.0523 0.8097 -0.2020 0.145 Uiso 1 1 calc R . . C15 C 0.1023(3) 0.7739(6) 0.2046(4) 0.0672(18) Uani 1 1 d . . . H15 H 0.0806 0.7100 0.1882 0.081 Uiso 1 1 calc R . . C16 C 0.0775(5) 0.8409(11) 0.2588(6) 0.144(5) Uani 1 1 d . . . H16A H 0.1005 0.8982 0.2818 0.216 Uiso 1 1 calc R . . H16B H 0.0706 0.7956 0.3000 0.216 Uiso 1 1 calc R . . H16C H 0.0457 0.8712 0.2287 0.216 Uiso 1 1 calc R . . C17 C 0.1539(4) 0.7357(9) 0.2510(6) 0.114(3) Uani 1 1 d . . . H17A H 0.1726 0.7956 0.2793 0.171 Uiso 1 1 calc R . . H17B H 0.1731 0.7060 0.2154 0.171 Uiso 1 1 calc R . . H17C H 0.1492 0.6810 0.2880 0.171 Uiso 1 1 calc R . . C18 C 0.2008(4) 0.4262(8) 0.2706(4) 0.091(3) Uani 1 1 d . . . H18A H 0.1881 0.4936 0.2860 0.137 Uiso 1 1 calc R . . H18B H 0.2371 0.4325 0.2732 0.137 Uiso 1 1 calc R . . H18C H 0.1951 0.3698 0.3057 0.137 Uiso 1 1 calc R . . C19 C 0.1954(4) 0.2690(7) 0.1379(6) 0.109(3) Uani 1 1 d . . . H19A H 0.2302 0.2840 0.1347 0.163 Uiso 1 1 calc R . . H19B H 0.1757 0.2452 0.0871 0.163 Uiso 1 1 calc R . . H19C H 0.1955 0.2132 0.1764 0.163 Uiso 1 1 calc R . . C20 C 0.0976(3) 0.3592(8) 0.1712(6) 0.104(3) Uani 1 1 d . . . H20A H 0.0780 0.3414 0.1189 0.157 Uiso 1 1 calc R . . H20B H 0.0823 0.4206 0.1908 0.157 Uiso 1 1 calc R . . H20C H 0.0977 0.2985 0.2058 0.157 Uiso 1 1 calc R . . C21 C 0.2677(3) 0.5935(9) 0.1453(6) 0.111(3) Uani 1 1 d . . . H21A H 0.2806 0.5328 0.1786 0.166 Uiso 1 1 calc R . . H21B H 0.2575 0.6499 0.1765 0.166 Uiso 1 1 calc R . . H21C H 0.2943 0.6200 0.1212 0.166 Uiso 1 1 calc R . . C22 C 0.2345(4) 0.4563(8) -0.0016(7) 0.107(3) Uani 1 1 d . . . H22A H 0.2055 0.4219 -0.0365 0.161 Uiso 1 1 calc R . . H22B H 0.2563 0.4022 0.0290 0.161 Uiso 1 1 calc R . . H22C H 0.2538 0.4965 -0.0322 0.161 Uiso 1 1 calc R . . C23 C 0.1842(3) 0.6718(6) 0.0060(5) 0.080(2) Uani 1 1 d . . . H23A H 0.1788 0.7291 0.0406 0.119 Uiso 1 1 calc R . . H23B H 0.1519 0.6534 -0.0295 0.119 Uiso 1 1 calc R . . H23C H 0.2082 0.6952 -0.0241 0.119 Uiso 1 1 calc R . . N1 N -0.00324(18) 0.5325(4) 0.0905(3) 0.0456(11) Uani 1 1 d . . . N2 N 0.04664(17) 0.7098(4) 0.0456(3) 0.0420(10) Uani 1 1 d . . . N3 N 0.16170(18) 0.4970(4) 0.1017(3) 0.0488(11) Uani 1 1 d . . . Nd1 Nd 0.077806(11) 0.54036(2) 0.040245(17) 0.04091(11) Uani 1 1 d . . . Si1 Si 0.16599(7) 0.39283(16) 0.16746(11) 0.0611(5) Uani 1 1 d . . . Si2 Si 0.21077(6) 0.55029(16) 0.06635(11) 0.0577(4) Uani 1 1 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 C1 0.061(4) 0.070(4) 0.043(3) -0.007(3) 0.020(3) -0.022(3) C2 0.060(4) 0.100(6) 0.059(4) -0.027(4) 0.032(3) -0.030(4) C3 0.050(4) 0.073(5) 0.072(4) -0.031(4) 0.025(3) -0.006(3) C4 0.043(3) 0.053(3) 0.057(3) -0.017(3) 0.016(3) -0.006(3) C5 0.045(3) 0.051(4) 0.090(5) -0.010(3) 0.013(3) -0.001(3) C6 0.044(3) 0.037(3) 0.053(3) -0.002(2) 0.017(3) -0.005(2) C7 0.063(4) 0.048(3) 0.052(3) 0.000(3) 0.023(3) 0.000(3) C8 0.097(6) 0.059(4) 0.087(5) 0.009(4) 0.044(5) -0.015(4) C9 0.097(6) 0.068(5) 0.110(7) -0.015(5) 0.038(6) -0.040(5) C10 0.075(5) 0.078(5) 0.078(5) -0.018(4) 0.015(4) -0.028(4) C11 0.052(3) 0.056(4) 0.056(4) -0.005(3) 0.016(3) -0.008(3) C12 0.095(5) 0.061(4) 0.044(3) 0.003(3) 0.021(3) 0.015(4) C13 0.111(7) 0.094(6) 0.071(5) 0.001(4) 0.012(5) 0.035(5) C14 0.128(8) 0.104(7) 0.063(5) 0.008(5) 0.032(5) 0.039(6) C15 0.075(5) 0.071(5) 0.050(4) 0.001(3) 0.002(3) -0.007(4) C16 0.170(11) 0.185(12) 0.100(7) 0.064(8) 0.078(8) 0.092(10) C17 0.098(7) 0.146(9) 0.093(6) 0.027(6) 0.015(5) 0.044(7) C18 0.096(6) 0.113(7) 0.058(4) 0.013(5) 0.005(4) 0.017(5) C19 0.158(10) 0.062(5) 0.098(7) 0.003(5) 0.015(6) 0.014(6) C20 0.087(6) 0.129(8) 0.095(6) 0.048(6) 0.016(5) -0.029(6) C21 0.062(5) 0.145(9) 0.113(7) 0.018(7) -0.006(5) -0.029(6) C22 0.097(7) 0.117(8) 0.131(8) 0.006(6) 0.074(7) 0.018(6) C23 0.070(5) 0.083(5) 0.090(5) 0.023(4) 0.028(4) -0.011(4) N1 0.047(3) 0.048(3) 0.045(3) -0.009(2) 0.017(2) -0.014(2) N2 0.041(2) 0.040(2) 0.047(2) -0.005(2) 0.014(2) -0.0044(19) N3 0.038(2) 0.057(3) 0.051(3) 0.001(2) 0.010(2) 0.002(2) Nd1 0.03798(17) 0.04208(18) 0.04394(18) -0.00378(13) 0.01215(12) -0.00502(13) Si1 0.0629(11) 0.0627(11) 0.0549(10) 0.0112(9) 0.0079(8) 0.0024(9) Si2 0.0377(8) 0.0695(12) 0.0672(11) 0.0051(9) 0.0148(8) -0.0019(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 C1 N1 1.370(7) . ? C1 C2 1.373(10) . ? C1 Nd1 2.760(6) 5_565 ? C2 C3 1.400(11) . ? C2 Nd1 2.816(6) 5_565 ? C3 C4 1.382(8) . ? C3 Nd1 2.883(6) 5_565 ? C4 N1 1.365(8) . ? C4 C5 1.504(9) . ? C4 Nd1 2.880(6) 5_565 ? C5 N2 1.451(7) . ? C6 C11 1.398(8) . ? C6 C7 1.404(8) . ? C6 N2 1.427(7) . ? C7 C8 1.381(9) . ? C7 C12 1.510(9) . ? C8 C9 1.359(12) . ? C9 C10 1.356(12) . ? C10 C11 1.393(9) . ? C11 C15 1.527(9) . ? C12 C14 1.521(10) . ? C12 C13 1.535(10) . ? C15 C17 1.496(10) . ? C15 C16 1.514(12) . ? C18 Si1 1.859(8) . ? C19 Si1 1.844(9) . ? C20 Si1 1.882(8) . ? C21 Si2 1.867(9) . ? C22 Si2 1.866(9) . ? C23 Si2 1.871(8) . ? N1 Nd1 2.511(4) . ? N1 Nd1 2.791(5) 5_565 ? N2 Nd1 2.259(4) . ? N3 Si2 1.701(5) . ? N3 Si1 1.705(5) . ? N3 Nd1 2.302(5) . ? Nd1 C1 2.760(6) 5_565 ? Nd1 N1 2.791(5) 5_565 ? Nd1 C2 2.816(6) 5_565 ? Nd1 C4 2.880(6) 5_565 ? Nd1 C3 2.883(6) 5_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.1(6) . . ? N1 C1 Nd1 77.0(3) . 5_565 ? C2 C1 Nd1 78.0(4) . 5_565 ? C1 C2 C3 107.1(6) . . ? C1 C2 Nd1 73.5(3) . 5_565 ? C3 C2 Nd1 78.4(4) . 5_565 ? C4 C3 C2 106.1(6) . . ? C4 C3 Nd1 76.0(3) . 5_565 ? C2 C3 Nd1 73.2(4) . 5_565 ? N1 C4 C3 110.5(6) . . ? N1 C4 C5 120.9(5) . . ? C3 C4 C5 128.2(6) . . ? N1 C4 Nd1 72.5(3) . 5_565 ? C3 C4 Nd1 76.2(3) . 5_565 ? C5 C4 Nd1 124.0(4) . 5_565 ? N2 C5 C4 112.3(5) . . ? C11 C6 C7 119.5(5) . . ? C11 C6 N2 119.8(5) . . ? C7 C6 N2 120.7(5) . . ? C8 C7 C6 119.1(6) . . ? C8 C7 C12 119.5(6) . . ? C6 C7 C12 121.4(6) . . ? C9 C8 C7 121.1(7) . . ? C10 C9 C8 120.4(7) . . ? C9 C10 C11 121.2(7) . . ? C10 C11 C6 118.6(6) . . ? C10 C11 C15 119.3(6) . . ? C6 C11 C15 122.0(5) . . ? C7 C12 C14 112.6(7) . . ? C7 C12 C13 111.6(6) . . ? C14 C12 C13 110.2(6) . . ? C17 C15 C16 108.5(7) . . ? C17 C15 C11 113.8(7) . . ? C16 C15 C11 110.7(6) . . ? C4 N1 C1 106.2(5) . . ? C4 N1 Nd1 110.3(3) . . ? C1 N1 Nd1 142.5(4) . . ? C4 N1 Nd1 79.7(3) . 5_565 ? C1 N1 Nd1 74.5(3) . 5_565 ? Nd1 N1 Nd1 103.62(15) . 5_565 ? C6 N2 C5 112.6(4) . . ? C6 N2 Nd1 126.8(3) . . ? C5 N2 Nd1 120.3(4) . . ? Si2 N3 Si1 126.6(3) . . ? Si2 N3 Nd1 119.1(3) . . ? Si1 N3 Nd1 113.1(2) . . ? N2 Nd1 N3 121.48(17) . . ? N2 Nd1 N1 70.60(15) . . ? N3 Nd1 N1 130.49(16) . . ? N2 Nd1 C1 89.00(19) . 5_565 ? N3 Nd1 C1 126.87(18) . 5_565 ? N1 Nd1 C1 98.96(17) . 5_565 ? N2 Nd1 N1 97.68(15) . 5_565 ? N3 Nd1 N1 136.90(16) . 5_565 ? N1 Nd1 N1 76.38(15) . 5_565 ? C1 Nd1 N1 28.57(15) 5_565 5_565 ? N2 Nd1 C2 109.7(2) . 5_565 ? N3 Nd1 C2 98.6(2) . 5_565 ? N1 Nd1 C2 123.62(17) . 5_565 ? C1 Nd1 C2 28.5(2) 5_565 5_565 ? N1 Nd1 C2 47.29(16) 5_565 5_565 ? N2 Nd1 C4 125.42(17) . 5_565 ? N3 Nd1 C4 111.27(17) . 5_565 ? N1 Nd1 C4 86.35(15) . 5_565 ? C1 Nd1 C4 45.56(19) 5_565 5_565 ? N1 Nd1 C4 27.81(15) 5_565 5_565 ? C2 Nd1 C4 45.93(19) 5_565 5_565 ? N2 Nd1 C3 135.3(2) . 5_565 ? N3 Nd1 C3 90.29(19) . 5_565 ? N1 Nd1 C3 114.01(16) . 5_565 ? C1 Nd1 C3 46.5(2) 5_565 5_565 ? N1 Nd1 C3 46.84(17) 5_565 5_565 ? C2 Nd1 C3 28.4(2) 5_565 5_565 ? C4 Nd1 C3 27.75(16) 5_565 5_565 ? N3 Si1 C19 113.9(4) . . ? N3 Si1 C18 114.7(4) . . ? C19 Si1 C18 107.7(4) . . ? N3 Si1 C20 106.0(3) . . ? C19 Si1 C20 107.6(5) . . ? C18 Si1 C20 106.5(4) . . ? N3 Si2 C22 112.9(4) . . ? N3 Si2 C21 114.0(4) . . ? C22 Si2 C21 107.7(5) . . ? N3 Si2 C23 106.9(3) . . ? C22 Si2 C23 106.5(4) . . ? C21 Si2 C23 108.5(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.763 _refine_diff_density_min -0.986 _refine_diff_density_rms 0.106 data_7b _database_code_depnum_ccdc_archive 'CCDC 896995' #TrackingRef 'CCDC 896995.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H80 N6 Si4 Sm2' _chemical_formula_weight 1130.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.5814(13) _cell_length_b 12.3473(6) _cell_length_c 17.3550(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.6210(10) _cell_angle_gamma 90.00 _cell_volume 5535.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9943 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.54 _exptl_crystal_description block _exptl_crystal_colour reddish _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 2.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5652 _exptl_absorpt_correction_T_max 0.7040 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21076 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.98 _reflns_number_total 5421 _reflns_number_gt 4608 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+5.7284P] 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 5421 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0588 _refine_ls_wR_factor_gt 0.0544 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 C1 C 1.03393(13) 0.4624(3) 0.88133(18) 0.0562(8) Uani 1 1 d . . . H1 H 1.0242 0.3936 0.8616 0.067 Uiso 1 1 calc R . . C2 C 1.08183(14) 0.5087(3) 0.8854(2) 0.0667(10) Uani 1 1 d . . . H2A H 1.1095 0.4772 0.8696 0.080 Uiso 1 1 calc R . . C3 C 1.08064(12) 0.6116(3) 0.9178(2) 0.0631(9) Uani 1 1 d . . . H3 H 1.1076 0.6616 0.9284 0.076 Uiso 1 1 calc R . . C4 C 1.03152(11) 0.6254(2) 0.93106(18) 0.0496(7) Uani 1 1 d . . . C5 C 1.00674(12) 0.7257(2) 0.9527(2) 0.0624(9) Uani 1 1 d . . . H5A H 1.0258 0.7504 1.0044 0.075 Uiso 1 1 calc R . . H5B H 1.0086 0.7821 0.9145 0.075 Uiso 1 1 calc R . . C6 C 0.92386(10) 0.8073(2) 0.94491(16) 0.0425(6) Uani 1 1 d . . . C7 C 0.92327(12) 0.8741(2) 1.00996(18) 0.0526(7) Uani 1 1 d . . . C8 C 0.89187(17) 0.9651(3) 0.9989(3) 0.0780(11) Uani 1 1 d . . . H8 H 0.8912 1.0095 1.0419 0.094 Uiso 1 1 calc R . . C9 C 0.86202(18) 0.9908(3) 0.9263(3) 0.0917(14) Uani 1 1 d . . . H9 H 0.8401 1.0505 0.9205 0.110 Uiso 1 1 calc R . . C10 C 0.86416(15) 0.9289(3) 0.8619(2) 0.0761(11) Uani 1 1 d . . . H10 H 0.8447 0.9491 0.8122 0.091 Uiso 1 1 calc R . . C11 C 0.89472(12) 0.8365(2) 0.86888(19) 0.0534(7) Uani 1 1 d . . . C12 C 0.95677(15) 0.8498(3) 1.09167(19) 0.0663(9) Uani 1 1 d . . . H12 H 0.9754 0.7823 1.0876 0.080 Uiso 1 1 calc R . . C13 C 0.99736(19) 0.9380(3) 1.1194(3) 0.0944(14) Uani 1 1 d . . . H13A H 0.9804 1.0058 1.1230 0.142 Uiso 1 1 calc R . . H13B H 1.0187 0.9446 1.0820 0.142 Uiso 1 1 calc R . . H13C H 1.0185 0.9191 1.1704 0.142 Uiso 1 1 calc R . . C14 C 0.92533(19) 0.8318(4) 1.1532(2) 0.0988(15) Uani 1 1 d . . . H14A H 0.9018 0.7725 1.1369 0.148 Uiso 1 1 calc R . . H14B H 0.9061 0.8962 1.1580 0.148 Uiso 1 1 calc R . . H14C H 0.9482 0.8152 1.2034 0.148 Uiso 1 1 calc R . . C15 C 0.89714(14) 0.7723(3) 0.79539(19) 0.0669(9) Uani 1 1 d . . . H15 H 0.9180 0.7074 0.8121 0.080 Uiso 1 1 calc R . . C16 C 0.9229(2) 0.8379(5) 0.7416(3) 0.159(3) Uani 1 1 d . . . H16A H 0.9014 0.8986 0.7208 0.239 Uiso 1 1 calc R . . H16B H 0.9278 0.7932 0.6987 0.239 Uiso 1 1 calc R . . H16C H 0.9559 0.8634 0.7714 0.239 Uiso 1 1 calc R . . C17 C 0.84538(18) 0.7374(4) 0.7476(3) 0.1170(18) Uani 1 1 d . . . H17A H 0.8265 0.7996 0.7230 0.175 Uiso 1 1 calc R . . H17B H 0.8265 0.7030 0.7816 0.175 Uiso 1 1 calc R . . H17C H 0.8499 0.6873 0.7075 0.175 Uiso 1 1 calc R . . C18 C 0.80050(18) 0.4273(4) 0.7299(2) 0.0886(12) Uani 1 1 d . . . H18A H 0.8141 0.4935 0.7140 0.133 Uiso 1 1 calc R . . H18B H 0.7642 0.4360 0.7273 0.133 Uiso 1 1 calc R . . H18C H 0.8053 0.3698 0.6951 0.133 Uiso 1 1 calc R . . C19 C 0.8052(2) 0.2695(3) 0.8625(3) 0.1066(16) Uani 1 1 d . . . H19A H 0.7695 0.2831 0.8612 0.160 Uiso 1 1 calc R . . H19B H 0.8231 0.2489 0.9152 0.160 Uiso 1 1 calc R . . H19C H 0.8077 0.2120 0.8263 0.160 Uiso 1 1 calc R . . C20 C 0.90329(16) 0.3582(4) 0.8293(3) 0.1076(17) Uani 1 1 d . . . H20A H 0.9225 0.3373 0.8811 0.161 Uiso 1 1 calc R . . H20B H 0.9195 0.4200 0.8117 0.161 Uiso 1 1 calc R . . H20C H 0.9027 0.2993 0.7930 0.161 Uiso 1 1 calc R . . C21 C 0.73375(15) 0.5931(4) 0.8551(3) 0.1075(16) Uani 1 1 d . . . H21A H 0.7216 0.5326 0.8211 0.161 Uiso 1 1 calc R . . H21B H 0.7438 0.6506 0.8246 0.161 Uiso 1 1 calc R . . H21C H 0.7066 0.6180 0.8787 0.161 Uiso 1 1 calc R . . C22 C 0.76629(19) 0.4568(4) 1.0018(3) 0.1037(16) Uani 1 1 d . . . H22A H 0.7950 0.4317 1.0424 0.156 Uiso 1 1 calc R . . H22B H 0.7494 0.3960 0.9720 0.156 Uiso 1 1 calc R . . H22C H 0.7422 0.4942 1.0257 0.156 Uiso 1 1 calc R . . C23 C 0.81568(14) 0.6743(3) 0.9935(2) 0.0781(11) Uani 1 1 d . . . H23A H 0.8207 0.7313 0.9585 0.117 Uiso 1 1 calc R . . H23B H 0.8481 0.6573 1.0294 0.117 Uiso 1 1 calc R . . H23C H 0.7913 0.6973 1.0231 0.117 Uiso 1 1 calc R . . N1 N 1.00276(9) 0.53215(18) 0.91049(14) 0.0454(6) Uani 1 1 d . . . N2 N 0.95269(8) 0.70853(17) 0.95439(13) 0.0422(5) Uani 1 1 d . . . N3 N 0.83965(9) 0.4978(2) 0.89882(14) 0.0465(5) Uani 1 1 d . . . Si1 Si 0.83506(4) 0.39378(8) 0.83314(6) 0.0598(2) Uani 1 1 d . . . Si2 Si 0.79019(3) 0.55112(7) 0.93397(6) 0.0567(2) Uani 1 1 d . . . Sm1 Sm 0.922882(5) 0.540192(11) 0.959851(8) 0.03866(6) Uani 1 1 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 C1 0.059(2) 0.068(2) 0.0438(17) 0.0084(14) 0.0161(15) 0.0228(16) C2 0.058(2) 0.092(3) 0.059(2) 0.0225(19) 0.0312(18) 0.0284(19) C3 0.0438(17) 0.077(2) 0.073(2) 0.0343(19) 0.0228(16) 0.0090(16) C4 0.0400(15) 0.0528(17) 0.0568(18) 0.0213(14) 0.0128(13) 0.0084(13) C5 0.0442(18) 0.0460(17) 0.095(3) 0.0124(17) 0.0129(17) 0.0040(14) C6 0.0398(15) 0.0392(14) 0.0494(16) 0.0034(12) 0.0123(13) 0.0026(11) C7 0.0604(19) 0.0451(16) 0.0559(18) -0.0006(14) 0.0210(15) -0.0011(14) C8 0.100(3) 0.056(2) 0.090(3) -0.008(2) 0.047(3) 0.015(2) C9 0.098(3) 0.067(2) 0.119(4) 0.017(3) 0.042(3) 0.043(2) C10 0.069(2) 0.075(2) 0.080(3) 0.020(2) 0.011(2) 0.027(2) C11 0.0468(17) 0.0549(18) 0.0577(19) 0.0096(14) 0.0105(15) 0.0118(14) C12 0.094(3) 0.060(2) 0.0481(18) -0.0070(15) 0.0219(18) -0.0164(18) C13 0.116(4) 0.089(3) 0.074(3) -0.003(2) 0.013(3) -0.041(3) C14 0.131(4) 0.108(3) 0.067(3) -0.011(2) 0.040(3) -0.044(3) C15 0.072(2) 0.073(2) 0.0493(19) -0.0008(16) 0.0006(17) 0.0053(18) C16 0.182(6) 0.209(7) 0.117(4) -0.081(4) 0.096(4) -0.117(5) C17 0.103(4) 0.145(5) 0.096(3) -0.026(3) 0.010(3) -0.045(3) C18 0.096(3) 0.105(3) 0.060(2) -0.012(2) 0.009(2) -0.013(3) C19 0.149(5) 0.060(2) 0.098(3) -0.001(2) 0.004(3) -0.019(3) C20 0.084(3) 0.129(4) 0.104(3) -0.060(3) 0.010(3) 0.032(3) C21 0.057(2) 0.141(4) 0.110(4) -0.021(3) -0.009(2) 0.031(3) C22 0.091(3) 0.113(4) 0.128(4) -0.004(3) 0.068(3) -0.019(3) C23 0.062(2) 0.078(2) 0.096(3) -0.021(2) 0.022(2) 0.0066(19) N1 0.0437(13) 0.0496(14) 0.0448(13) 0.0090(10) 0.0141(11) 0.0137(11) N2 0.0367(12) 0.0409(12) 0.0485(13) 0.0049(10) 0.0088(10) 0.0063(10) N3 0.0369(13) 0.0518(13) 0.0496(14) -0.0016(11) 0.0082(11) 0.0012(10) Si1 0.0584(6) 0.0601(6) 0.0568(5) -0.0109(4) 0.0050(4) -0.0011(4) Si2 0.0351(4) 0.0669(6) 0.0682(6) -0.0061(4) 0.0126(4) 0.0015(4) Sm1 0.03266(8) 0.03910(9) 0.04400(9) 0.00406(6) 0.00856(6) 0.00550(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.372(4) . ? C1 C2 1.382(5) . ? C1 Sm1 2.725(3) 5_767 ? C2 C3 1.392(5) . ? C2 Sm1 2.783(3) 5_767 ? C3 C4 1.389(4) . ? C3 Sm1 2.851(3) 5_767 ? C4 N1 1.382(4) . ? C4 C5 1.492(4) . ? C4 Sm1 2.855(3) 5_767 ? C5 N2 1.460(4) . ? C6 C7 1.402(4) . ? C6 C11 1.411(4) . ? C6 N2 1.429(3) . ? C7 C8 1.385(5) . ? C7 C12 1.516(5) . ? C8 C9 1.358(6) . ? C9 C10 1.367(6) . ? C10 C11 1.389(4) . ? C11 C15 1.516(4) . ? C12 C14 1.519(5) . ? C12 C13 1.529(5) . ? C15 C17 1.493(5) . ? C15 C16 1.516(6) . ? C18 Si1 1.857(4) . ? C19 Si1 1.853(4) . ? C20 Si1 1.883(4) . ? C21 Si2 1.851(4) . ? C22 Si2 1.870(4) . ? C23 Si2 1.873(4) . ? N1 Sm1 2.472(2) . ? N1 Sm1 2.770(2) 5_767 ? N2 Sm1 2.234(2) . ? N3 Si1 1.702(3) . ? N3 Si2 1.707(2) . ? N3 Sm1 2.278(2) . ? Si1 Sm1 3.3371(9) . ? Si2 Sm1 3.4518(9) . ? Sm1 C1 2.725(3) 5_767 ? Sm1 N1 2.770(2) 5_767 ? Sm1 C2 2.783(3) 5_767 ? Sm1 C3 2.851(3) 5_767 ? Sm1 C4 2.855(3) 5_767 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.5(3) . . ? N1 C1 Sm1 77.37(16) . 5_767 ? C2 C1 Sm1 77.8(2) . 5_767 ? C1 C2 C3 106.9(3) . . ? C1 C2 Sm1 73.14(18) . 5_767 ? C3 C2 Sm1 78.39(19) . 5_767 ? C4 C3 C2 106.9(3) . . ? C4 C3 Sm1 76.10(16) . 5_767 ? C2 C3 Sm1 73.02(18) . 5_767 ? N1 C4 C3 109.8(3) . . ? N1 C4 C5 120.5(2) . . ? C3 C4 C5 129.2(3) . . ? N1 C4 Sm1 72.37(14) . 5_767 ? C3 C4 Sm1 75.72(17) . 5_767 ? C5 C4 Sm1 124.9(2) . 5_767 ? N2 C5 C4 112.3(2) . . ? C7 C6 C11 119.7(3) . . ? C7 C6 N2 121.1(3) . . ? C11 C6 N2 119.2(2) . . ? C8 C7 C6 119.1(3) . . ? C8 C7 C12 119.5(3) . . ? C6 C7 C12 121.4(3) . . ? C9 C8 C7 121.3(4) . . ? C8 C9 C10 120.0(4) . . ? C9 C10 C11 121.6(4) . . ? C10 C11 C6 118.2(3) . . ? C10 C11 C15 119.7(3) . . ? C6 C11 C15 122.1(3) . . ? C7 C12 C14 112.8(3) . . ? C7 C12 C13 111.6(3) . . ? C14 C12 C13 110.4(3) . . ? C17 C15 C11 113.7(3) . . ? C17 C15 C16 107.7(4) . . ? C11 C15 C16 110.7(3) . . ? C1 N1 C4 105.9(3) . . ? C1 N1 Sm1 142.7(2) . . ? C4 N1 Sm1 110.19(17) . . ? C1 N1 Sm1 73.73(16) . 5_767 ? C4 N1 Sm1 79.25(16) . 5_767 ? Sm1 N1 Sm1 103.78(8) . 5_767 ? C6 N2 C5 112.2(2) . . ? C6 N2 Sm1 127.79(17) . . ? C5 N2 Sm1 119.79(17) . . ? Si1 N3 Si2 126.21(15) . . ? Si1 N3 Sm1 113.18(12) . . ? Si2 N3 Sm1 119.39(13) . . ? N3 Si1 C19 114.12(18) . . ? N3 Si1 C18 114.77(17) . . ? C19 Si1 C18 107.7(2) . . ? N3 Si1 C20 106.38(16) . . ? C19 Si1 C20 107.1(2) . . ? C18 Si1 C20 106.2(2) . . ? N3 Si1 Sm1 38.86(8) . . ? C19 Si1 Sm1 123.07(15) . . ? C18 Si1 Sm1 128.69(14) . . ? C20 Si1 Sm1 67.64(13) . . ? N3 Si2 C21 113.73(18) . . ? N3 Si2 C22 112.89(17) . . ? C21 Si2 C22 107.7(2) . . ? N3 Si2 C23 107.54(15) . . ? C21 Si2 C23 107.8(2) . . ? C22 Si2 C23 106.9(2) . . ? N3 Si2 Sm1 35.09(8) . . ? C21 Si2 Sm1 137.11(17) . . ? C22 Si2 Sm1 112.45(17) . . ? C23 Si2 Sm1 74.58(11) . . ? N2 Sm1 N3 120.64(8) . . ? N2 Sm1 N1 71.37(8) . . ? N3 Sm1 N1 130.49(8) . . ? N2 Sm1 C1 89.12(9) . 5_767 ? N3 Sm1 C1 126.83(9) . 5_767 ? N1 Sm1 C1 99.11(9) . 5_767 ? N2 Sm1 N1 98.17(8) . 5_767 ? N3 Sm1 N1 137.12(8) . 5_767 ? N1 Sm1 N1 76.22(8) . 5_767 ? C1 Sm1 N1 28.89(7) 5_767 5_767 ? N2 Sm1 C2 109.85(11) . 5_767 ? N3 Sm1 C2 98.01(10) . 5_767 ? N1 Sm1 C2 124.27(9) . 5_767 ? C1 Sm1 C2 29.04(10) 5_767 5_767 ? N1 Sm1 C2 48.09(8) 5_767 5_767 ? N2 Sm1 C3 135.84(10) . 5_767 ? N3 Sm1 C3 89.80(9) . 5_767 ? N1 Sm1 C3 114.42(8) . 5_767 ? C1 Sm1 C3 47.05(11) 5_767 5_767 ? N1 Sm1 C3 47.55(8) 5_767 5_767 ? C2 Sm1 C3 28.58(11) 5_767 5_767 ? N2 Sm1 C4 126.50(9) . 5_767 ? N3 Sm1 C4 110.97(9) . 5_767 ? N1 Sm1 C4 86.32(8) . 5_767 ? C1 Sm1 C4 46.29(10) 5_767 5_767 ? N1 Sm1 C4 28.38(8) 5_767 5_767 ? C2 Sm1 C4 46.65(9) 5_767 5_767 ? C3 Sm1 C4 28.17(8) 5_767 5_767 ? N2 Sm1 Si1 132.53(6) . . ? N3 Sm1 Si1 27.96(6) . . ? N1 Sm1 Si1 105.94(6) . . ? C1 Sm1 Si1 136.29(8) 5_767 . ? N1 Sm1 Si1 127.97(5) 5_767 . ? C2 Sm1 Si1 109.56(9) 5_767 . ? C3 Sm1 Si1 89.67(8) 5_767 . ? C4 Sm1 Si1 99.84(7) 5_767 . ? N2 Sm1 Si2 108.65(6) . . ? N3 Sm1 Si2 25.52(6) . . ? N1 Sm1 Si2 153.05(6) . . ? C1 Sm1 Si2 107.84(7) 5_767 . ? N1 Sm1 Si2 129.06(5) 5_767 . ? C2 Sm1 Si2 81.80(7) 5_767 . ? C3 Sm1 Si2 84.89(6) 5_767 . ? C4 Sm1 Si2 112.06(6) 5_767 . ? Si1 Sm1 Si2 53.17(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.562 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.066 data_7c _database_code_depnum_ccdc_archive 'CCDC 896996' #TrackingRef 'CCDC 896996.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H80 Er2 N6 Si4' _chemical_formula_weight 1164.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.377(5) _cell_length_b 19.276(4) _cell_length_c 12.747(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.327(3) _cell_angle_gamma 90.00 _cell_volume 5391(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9963 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 26.97 _exptl_crystal_description block _exptl_crystal_colour reddish _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 3.215 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5953 _exptl_absorpt_correction_T_max 0.6989 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39994 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.0691 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10566 _reflns_number_gt 7411 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Restraints have been applied to refine the isopropyl group which is affected by disorder. DELU 0.01 C15 C16 C17 SIMU 0.01 C15 C16 C17 ; _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^)+(0.0469P)^2^+6.5971P] 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 10566 _refine_ls_number_parameters 543 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.0992 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.040 _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 C1 C 0.4437(4) 0.1052(4) 0.0123(6) 0.057(2) Uani 1 1 d . . . H1 H 0.4540 0.1401 -0.0312 0.068 Uiso 1 1 calc R . . C2 C 0.3860(4) 0.0913(5) 0.0259(6) 0.064(2) Uani 1 1 d . . . H2 H 0.3507 0.1138 -0.0079 0.077 Uiso 1 1 calc R . . C3 C 0.3895(3) 0.0368(5) 0.1001(6) 0.063(2) Uani 1 1 d . . . H3 H 0.3573 0.0173 0.1261 0.075 Uiso 1 1 calc R . . C4 C 0.4497(3) 0.0179(5) 0.1265(5) 0.055(2) Uani 1 1 d . . . C5 C 0.4808(4) -0.0300(5) 0.2114(7) 0.064(2) Uani 1 1 d . . . H5A H 0.4698 -0.0173 0.2787 0.076 Uiso 1 1 calc R . . H5B H 0.4663 -0.0768 0.1940 0.076 Uiso 1 1 calc R . . C6 C 0.5740(3) -0.0543(5) 0.3314(6) 0.053(2) Uani 1 1 d . . . C7 C 0.5808(4) -0.1268(6) 0.3495(7) 0.070(3) Uani 1 1 d . . . C8 C 0.6083(4) -0.1479(7) 0.4541(9) 0.092(4) Uani 1 1 d . . . H8 H 0.6137 -0.1950 0.4684 0.110 Uiso 1 1 calc R . . C9 C 0.6269(5) -0.1024(9) 0.5335(9) 0.105(5) Uani 1 1 d . . . H9 H 0.6444 -0.1181 0.6015 0.126 Uiso 1 1 calc R . . C10 C 0.6202(5) -0.0324(7) 0.5141(8) 0.096(4) Uani 1 1 d . . . H10 H 0.6343 -0.0016 0.5694 0.115 Uiso 1 1 calc R . . C11 C 0.5926(4) -0.0058(6) 0.4134(7) 0.068(3) Uani 1 1 d . . . C12 C 0.5579(5) -0.1809(5) 0.2659(9) 0.084(3) Uani 1 1 d . . . H12 H 0.5412 -0.1562 0.1994 0.101 Uiso 1 1 calc R . . C13 C 0.5071(6) -0.2252(6) 0.2927(10) 0.117(4) Uani 1 1 d . . . H13A H 0.4737 -0.1961 0.3020 0.176 Uiso 1 1 calc R . . H13B H 0.5218 -0.2503 0.3577 0.176 Uiso 1 1 calc R . . H13C H 0.4935 -0.2574 0.2355 0.176 Uiso 1 1 calc R . . C14 C 0.6113(7) -0.2262(7) 0.2442(12) 0.153(6) Uani 1 1 d . . . H14A H 0.5958 -0.2616 0.1931 0.229 Uiso 1 1 calc R . . H14B H 0.6315 -0.2474 0.3097 0.229 Uiso 1 1 calc R . . H14C H 0.6397 -0.1977 0.2162 0.229 Uiso 1 1 calc R . . C15 C 0.5830(5) 0.0713(6) 0.3970(9) 0.088(3) Uani 1 1 d U . . H15 H 0.5688 0.0798 0.3203 0.106 Uiso 1 1 calc R . . C16 C 0.5364(6) 0.0999(7) 0.4552(13) 0.150(5) Uani 1 1 d U . . H16A H 0.5445 0.0830 0.5274 0.225 Uiso 1 1 calc R . . H16B H 0.4965 0.0854 0.4198 0.225 Uiso 1 1 calc R . . H16C H 0.5385 0.1496 0.4557 0.225 Uiso 1 1 calc R . . C17 C 0.6413(5) 0.1123(7) 0.4337(11) 0.129(4) Uani 1 1 d U . . H17A H 0.6499 0.1152 0.5104 0.194 Uiso 1 1 calc R . . H17B H 0.6364 0.1581 0.4039 0.194 Uiso 1 1 calc R . . H17C H 0.6744 0.0894 0.4101 0.194 Uiso 1 1 calc R . . C18 C 0.6780(7) 0.2212(6) 0.1991(10) 0.139(5) Uani 1 1 d . . . H18A H 0.7136 0.2097 0.2515 0.209 Uiso 1 1 calc R . . H18B H 0.6429 0.2207 0.2319 0.209 Uiso 1 1 calc R . . H18C H 0.6828 0.2666 0.1709 0.209 Uiso 1 1 calc R . . C19 C 0.7248(5) 0.1779(6) 0.0060(10) 0.120(5) Uani 1 1 d . . . H19A H 0.7179 0.1494 -0.0570 0.181 Uiso 1 1 calc R . . H19B H 0.7651 0.1694 0.0465 0.181 Uiso 1 1 calc R . . H19C H 0.7211 0.2259 -0.0144 0.181 Uiso 1 1 calc R . . C20 C 0.5905(5) 0.1735(6) 0.0077(10) 0.117(4) Uani 1 1 d . . . H20A H 0.5603 0.1589 0.0470 0.175 Uiso 1 1 calc R . . H20B H 0.5855 0.1480 -0.0581 0.175 Uiso 1 1 calc R . . H20C H 0.5859 0.2222 -0.0075 0.175 Uiso 1 1 calc R . . C21 C 0.7881(4) 0.0777(7) 0.2872(8) 0.104(4) Uani 1 1 d . . . H21A H 0.7676 0.0916 0.3432 0.155 Uiso 1 1 calc R . . H21B H 0.8022 0.1180 0.2552 0.155 Uiso 1 1 calc R . . H21C H 0.8223 0.0488 0.3167 0.155 Uiso 1 1 calc R . . C22 C 0.7787(4) 0.0013(5) 0.0801(7) 0.072(3) Uani 1 1 d . . . H22A H 0.7936 0.0419 0.0498 0.108 Uiso 1 1 calc R . . H22B H 0.7528 -0.0245 0.0246 0.108 Uiso 1 1 calc R . . H22C H 0.8125 -0.0271 0.1127 0.108 Uiso 1 1 calc R . . C23 C 0.7122(4) -0.0535(6) 0.2440(8) 0.087(3) Uani 1 1 d . . . H23A H 0.6838 -0.0788 0.1916 0.131 Uiso 1 1 calc R . . H23B H 0.6935 -0.0424 0.3036 0.131 Uiso 1 1 calc R . . H23C H 0.7478 -0.0813 0.2681 0.131 Uiso 1 1 calc R . . C1' C 0.9370(3) 0.4417(3) 0.6081(5) 0.0362(15) Uani 1 1 d . . . H1' H 0.9254 0.3978 0.5815 0.043 Uiso 1 1 calc R . . C2' C 0.9540(3) 0.4571(4) 0.7140(5) 0.0448(17) Uani 1 1 d . . . H2' H 0.9563 0.4264 0.7708 0.054 Uiso 1 1 calc R . . C3' C 0.9677(3) 0.5289(4) 0.7213(5) 0.0448(18) Uani 1 1 d . . . H3' H 0.9813 0.5544 0.7833 0.054 Uiso 1 1 calc R . . C4' C 0.9566(3) 0.5537(3) 0.6163(5) 0.0329(14) Uani 1 1 d . . . C5' C 0.9526(3) 0.6272(3) 0.5777(5) 0.0390(16) Uani 1 1 d . . . H5'1 H 0.9217 0.6515 0.6072 0.047 Uiso 1 1 calc R . . H5'2 H 0.9913 0.6502 0.6033 0.047 Uiso 1 1 calc R . . C6' C 0.9185(3) 0.7000(3) 0.4248(5) 0.0356(15) Uani 1 1 d . . . C7' C 0.9615(3) 0.7500(4) 0.4091(5) 0.0414(16) Uani 1 1 d . . . C8' C 0.9401(4) 0.8120(4) 0.3610(6) 0.056(2) Uani 1 1 d . . . H8' H 0.9684 0.8447 0.3482 0.067 Uiso 1 1 calc R . . C9' C 0.8801(4) 0.8274(4) 0.3317(6) 0.062(2) Uani 1 1 d . . . H9' H 0.8675 0.8696 0.2994 0.074 Uiso 1 1 calc R . . C10' C 0.8382(4) 0.7791(4) 0.3509(6) 0.053(2) Uani 1 1 d . . . H10' H 0.7968 0.7891 0.3308 0.064 Uiso 1 1 calc R . . C11' C 0.8560(3) 0.7154(3) 0.3998(5) 0.0408(16) Uani 1 1 d . . . C12' C 1.0294(3) 0.7387(4) 0.4435(6) 0.0456(17) Uani 1 1 d . . . H12' H 1.0354 0.6922 0.4748 0.055 Uiso 1 1 calc R . . C13' C 1.0575(4) 0.7906(4) 0.5307(7) 0.066(2) Uani 1 1 d . . . H13D H 1.0499 0.8370 0.5042 0.099 Uiso 1 1 calc R . . H13E H 1.1007 0.7829 0.5499 0.099 Uiso 1 1 calc R . . H13F H 1.0396 0.7843 0.5925 0.099 Uiso 1 1 calc R . . C14' C 1.0623(4) 0.7410(5) 0.3494(7) 0.068(2) Uani 1 1 d . . . H14D H 1.0463 0.7055 0.2989 0.103 Uiso 1 1 calc R . . H14E H 1.1051 0.7334 0.3748 0.103 Uiso 1 1 calc R . . H14F H 1.0562 0.7856 0.3154 0.103 Uiso 1 1 calc R . . C15' C 0.8082(3) 0.6681(4) 0.4276(6) 0.0532(19) Uani 1 1 d . . . H15' H 0.8280 0.6243 0.4534 0.064 Uiso 1 1 calc R . . C16' C 0.7802(4) 0.6985(5) 0.5173(8) 0.080(3) Uani 1 1 d . . . H16D H 0.8120 0.7109 0.5764 0.120 Uiso 1 1 calc R . . H16E H 0.7540 0.6647 0.5403 0.120 Uiso 1 1 calc R . . H16F H 0.7569 0.7390 0.4917 0.120 Uiso 1 1 calc R . . C17' C 0.7583(4) 0.6518(5) 0.3322(8) 0.085(3) Uani 1 1 d . . . H17D H 0.7370 0.6937 0.3071 0.127 Uiso 1 1 calc R . . H17E H 0.7303 0.6193 0.3529 0.127 Uiso 1 1 calc R . . H17F H 0.7760 0.6322 0.2761 0.127 Uiso 1 1 calc R . . C18' C 0.8634(4) 0.3854(5) 0.3481(7) 0.082(3) Uani 1 1 d . . . H18D H 0.9048 0.3760 0.3422 0.123 Uiso 1 1 calc R . . H18E H 0.8413 0.3425 0.3455 0.123 Uiso 1 1 calc R . . H18F H 0.8630 0.4084 0.4147 0.123 Uiso 1 1 calc R . . C19' C 0.8156(4) 0.3895(5) 0.1089(6) 0.067(2) Uani 1 1 d . . . H19D H 0.7966 0.4172 0.0491 0.101 Uiso 1 1 calc R . . H19E H 0.7901 0.3503 0.1159 0.101 Uiso 1 1 calc R . . H19F H 0.8545 0.3735 0.0977 0.101 Uiso 1 1 calc R . . C20' C 0.7493(4) 0.4640(4) 0.2567(7) 0.062(2) Uani 1 1 d . . . H20D H 0.7521 0.4797 0.3290 0.093 Uiso 1 1 calc R . . H20E H 0.7240 0.4235 0.2448 0.093 Uiso 1 1 calc R . . H20F H 0.7318 0.5000 0.2081 0.093 Uiso 1 1 calc R . . C21' C 0.9158(4) 0.5195(5) 0.0261(6) 0.066(2) Uani 1 1 d . . . H21D H 0.9552 0.5060 0.0656 0.100 Uiso 1 1 calc R . . H21E H 0.9208 0.5512 -0.0296 0.100 Uiso 1 1 calc R . . H21F H 0.8942 0.4791 -0.0050 0.100 Uiso 1 1 calc R . . C22' C 0.7933(4) 0.5824(5) 0.0444(6) 0.066(2) Uani 1 1 d . . . H22D H 0.7744 0.5404 0.0138 0.100 Uiso 1 1 calc R . . H22E H 0.7955 0.6151 -0.0115 0.100 Uiso 1 1 calc R . . H22F H 0.7697 0.6018 0.0924 0.100 Uiso 1 1 calc R . . C23' C 0.9097(4) 0.6474(5) 0.1584(6) 0.066(2) Uani 1 1 d . . . H23D H 0.8873 0.6726 0.2029 0.099 Uiso 1 1 calc R . . H23E H 0.9113 0.6741 0.0953 0.099 Uiso 1 1 calc R . . H23F H 0.9504 0.6391 0.1971 0.099 Uiso 1 1 calc R . . Er1 Er 0.583368(14) 0.01257(2) 0.09240(2) 0.04591(11) Uani 1 1 d . . . Er1' Er 0.944358(13) 0.536202(15) 0.37154(2) 0.03095(9) Uani 1 1 d . . . N1 N 0.4849(3) 0.0599(3) 0.0726(4) 0.0466(15) Uani 1 1 d . . . N2 N 0.5475(3) -0.0294(3) 0.2250(5) 0.0467(15) Uani 1 1 d . . . N3 N 0.6692(3) 0.0726(3) 0.1301(4) 0.0505(16) Uani 1 1 d . . . N1' N 0.9392(2) 0.4994(3) 0.5458(4) 0.0315(12) Uani 1 1 d . . . N2' N 0.9376(2) 0.6311(3) 0.4612(4) 0.0317(12) Uani 1 1 d . . . N3' N 0.8717(3) 0.5142(3) 0.2322(4) 0.0406(14) Uani 1 1 d . . . Si1 Si 0.66777(11) 0.15667(14) 0.0888(2) 0.0644(6) Uani 1 1 d . . . Si2 Si 0.73424(10) 0.02794(14) 0.18335(17) 0.0578(6) Uani 1 1 d . . . Si1' Si 0.82648(9) 0.44270(12) 0.23377(15) 0.0453(5) Uani 1 1 d . . . Si2' Si 0.87136(9) 0.56300(12) 0.11908(15) 0.0466(5) Uani 1 1 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 C1 0.060(5) 0.056(5) 0.051(5) -0.001(4) 0.003(4) 0.011(4) C2 0.048(5) 0.085(7) 0.058(5) -0.003(5) 0.006(4) 0.026(5) C3 0.038(4) 0.113(8) 0.040(4) -0.005(4) 0.015(3) 0.010(5) C4 0.036(4) 0.100(7) 0.028(3) 0.000(4) 0.006(3) -0.001(4) C5 0.047(5) 0.092(7) 0.050(5) 0.011(4) 0.006(4) -0.005(4) C6 0.034(4) 0.079(6) 0.047(4) 0.017(4) 0.011(3) -0.005(4) C7 0.045(5) 0.093(8) 0.075(6) 0.032(5) 0.020(4) 0.005(5) C8 0.062(7) 0.129(10) 0.083(8) 0.051(7) 0.009(6) 0.015(6) C9 0.066(7) 0.174(14) 0.067(7) 0.056(8) -0.006(6) 0.002(8) C10 0.062(7) 0.170(13) 0.049(6) 0.017(7) -0.006(5) -0.034(7) C11 0.036(5) 0.113(8) 0.055(5) -0.001(5) 0.010(4) -0.012(5) C12 0.099(8) 0.066(7) 0.094(8) 0.013(6) 0.035(6) 0.014(6) C13 0.132(11) 0.100(10) 0.119(10) 0.023(8) 0.022(8) -0.024(8) C14 0.161(14) 0.119(12) 0.201(17) -0.002(11) 0.092(12) 0.038(10) C15 0.089(7) 0.095(8) 0.087(7) -0.008(6) 0.032(5) -0.019(6) C16 0.118(9) 0.131(11) 0.223(13) -0.010(10) 0.088(9) 0.001(8) C17 0.097(8) 0.130(10) 0.163(11) -0.014(9) 0.032(8) -0.034(7) C18 0.209(16) 0.080(9) 0.125(11) -0.024(8) 0.023(10) -0.008(10) C19 0.130(11) 0.104(10) 0.147(12) 0.041(8) 0.077(9) -0.006(8) C20 0.085(8) 0.083(8) 0.165(12) 0.027(8) -0.016(8) 0.011(7) C21 0.059(6) 0.158(12) 0.080(7) -0.033(7) -0.020(5) 0.004(7) C22 0.046(5) 0.105(8) 0.070(6) 0.003(5) 0.021(4) 0.005(5) C23 0.062(6) 0.128(9) 0.075(6) 0.032(6) 0.022(5) 0.034(6) C1' 0.035(4) 0.029(4) 0.046(4) 0.011(3) 0.012(3) -0.002(3) C2' 0.054(5) 0.044(5) 0.041(4) 0.010(3) 0.022(3) 0.007(3) C3' 0.063(5) 0.046(5) 0.027(3) 0.000(3) 0.014(3) 0.007(4) C4' 0.039(4) 0.026(4) 0.034(3) 0.000(3) 0.008(3) 0.002(3) C5' 0.045(4) 0.038(4) 0.033(3) 0.001(3) 0.006(3) 0.004(3) C6' 0.052(4) 0.026(4) 0.030(3) 0.001(3) 0.010(3) 0.003(3) C7' 0.055(5) 0.037(4) 0.034(3) 0.002(3) 0.013(3) -0.002(3) C8' 0.083(6) 0.033(4) 0.054(5) 0.015(3) 0.017(4) -0.005(4) C9' 0.087(7) 0.036(5) 0.060(5) 0.015(4) 0.009(5) 0.010(4) C10' 0.060(5) 0.043(5) 0.053(5) 0.005(4) 0.004(4) 0.017(4) C11' 0.048(4) 0.028(4) 0.047(4) 0.001(3) 0.009(3) 0.003(3) C12' 0.049(4) 0.043(4) 0.047(4) 0.003(3) 0.016(3) -0.009(3) C13' 0.068(6) 0.064(6) 0.066(6) -0.010(4) 0.014(4) -0.019(5) C14' 0.071(6) 0.077(6) 0.065(6) -0.002(5) 0.033(5) -0.011(5) C15' 0.048(5) 0.043(5) 0.069(5) -0.002(4) 0.012(4) 0.004(4) C16' 0.077(7) 0.081(7) 0.092(7) -0.004(5) 0.041(6) -0.015(5) C17' 0.063(6) 0.085(8) 0.102(8) -0.023(6) 0.004(5) -0.015(5) C18' 0.076(7) 0.094(8) 0.067(6) 0.029(5) -0.005(5) -0.003(6) C19' 0.091(7) 0.060(6) 0.047(5) -0.015(4) 0.003(4) -0.002(5) C20' 0.049(5) 0.069(6) 0.067(5) 0.000(4) 0.010(4) -0.008(4) C21' 0.081(6) 0.089(7) 0.033(4) -0.004(4) 0.019(4) 0.007(5) C22' 0.067(6) 0.083(7) 0.045(4) 0.009(4) 0.001(4) 0.006(5) C23' 0.069(6) 0.076(6) 0.051(5) 0.001(4) 0.007(4) -0.012(5) Er1 0.03149(18) 0.0693(3) 0.03638(18) 0.00217(15) 0.00531(13) 0.00170(16) Er1' 0.03421(17) 0.03068(16) 0.02715(14) -0.00065(11) 0.00406(11) 0.00243(13) N1 0.037(3) 0.065(4) 0.039(3) -0.004(3) 0.009(3) 0.006(3) N2 0.036(3) 0.063(4) 0.041(3) 0.005(3) 0.006(3) 0.003(3) N3 0.035(3) 0.072(5) 0.044(3) 0.001(3) 0.009(3) -0.003(3) N1' 0.027(3) 0.026(3) 0.045(3) 0.000(2) 0.013(2) 0.002(2) N2' 0.039(3) 0.026(3) 0.031(3) 0.001(2) 0.009(2) 0.003(2) N3' 0.040(3) 0.056(4) 0.024(3) 0.003(2) 0.001(2) 0.002(3) Si1 0.0566(15) 0.0675(17) 0.0684(16) -0.0006(12) 0.0110(12) -0.0061(12) Si2 0.0371(12) 0.0947(19) 0.0414(11) 0.0038(11) 0.0071(9) 0.0027(11) Si1' 0.0426(12) 0.0561(13) 0.0344(10) -0.0013(9) 0.0010(8) 0.0003(10) Si2' 0.0434(12) 0.0637(14) 0.0312(10) 0.0015(9) 0.0033(8) -0.0010(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.362(11) . ? C1 N1 1.386(9) . ? C1 Er1 2.643(8) 3_655 ? C1 H1 0.9300 . ? C2 C3 1.406(12) . ? C2 Er1 2.676(8) 3_655 ? C2 H2 0.9300 . ? C3 C4 1.372(10) . ? C3 Er1 2.807(7) 3_655 ? C3 H3 0.9300 . ? C4 N1 1.400(9) . ? C4 C5 1.487(11) . ? C4 Er1 2.805(7) 3_655 ? C5 N2 1.467(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C11 1.402(12) . ? C6 C7 1.420(12) . ? C6 N2 1.451(9) . ? C7 C8 1.414(12) . ? C7 C12 1.506(14) . ? C8 C9 1.343(16) . ? C8 H8 0.9300 . ? C9 C10 1.373(16) . ? C9 H9 0.9300 . ? C10 C11 1.407(13) . ? C10 H10 0.9300 . ? C11 C15 1.512(14) . ? C12 C13 1.514(14) . ? C12 C14 1.550(14) . ? C12 H12 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.497(14) . ? C15 C17 1.518(14) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 Si1 1.857(11) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 Si1 1.855(10) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 Si1 1.860(10) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 Si2 1.871(9) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 Si2 1.871(8) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 Si2 1.858(10) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C1' C2' 1.361(9) . ? C1' N1' 1.374(8) . ? C1' Er1' 2.650(6) 3_766 ? C1' H1' 0.9300 . ? C2' C3' 1.416(10) . ? C2' Er1' 2.711(7) 3_766 ? C2' H2' 0.9300 . ? C3' C4' 1.396(9) . ? C3' Er1' 2.786(7) 3_766 ? C3' H3' 0.9300 . ? C4' N1' 1.384(8) . ? C4' C5' 1.498(9) . ? C4' Er1' 2.792(6) 3_766 ? C5' N2' 1.459(7) . ? C5' H5'1 0.9700 . ? C5' H5'2 0.9700 . ? C6' C7' 1.402(9) . ? C6' C11' 1.405(9) . ? C6' N2' 1.444(8) . ? C7' C8' 1.385(10) . ? C7' C12' 1.513(10) . ? C8' C9' 1.354(11) . ? C8' H8' 0.9300 . ? C9' C10' 1.377(11) . ? C9' H9' 0.9300 . ? C10' C11' 1.399(9) . ? C10' H10' 0.9300 . ? C11' C15' 1.500(10) . ? C12' C14' 1.526(9) . ? C12' C13' 1.535(10) . ? C12' H12' 0.9800 . ? C13' H13D 0.9600 . ? C13' H13E 0.9600 . ? C13' H13F 0.9600 . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15' C17' 1.513(11) . ? C15' C16' 1.525(11) . ? C15' H15' 0.9800 . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17' H17D 0.9600 . ? C17' H17E 0.9600 . ? C17' H17F 0.9600 . ? C18' Si1' 1.885(8) . ? C18' H18D 0.9600 . ? C18' H18E 0.9600 . ? C18' H18F 0.9600 . ? C19' Si1' 1.869(7) . ? C19' H19D 0.9600 . ? C19' H19E 0.9600 . ? C19' H19F 0.9600 . ? C20' Si1' 1.853(8) . ? C20' H20D 0.9600 . ? C20' H20E 0.9600 . ? C20' H20F 0.9600 . ? C21' Si2' 1.887(8) . ? C21' H21D 0.9600 . ? C21' H21E 0.9600 . ? C21' H21F 0.9600 . ? C22' Si2' 1.855(8) . ? C22' H22D 0.9600 . ? C22' H22E 0.9600 . ? C22' H22F 0.9600 . ? C23' Si2' 1.862(9) . ? C23' H23D 0.9600 . ? C23' H23E 0.9600 . ? C23' H23F 0.9600 . ? Er1 N2 2.166(6) . ? Er1 N3 2.213(6) . ? Er1 N1 2.353(6) . ? Er1 C1 2.643(8) 3_655 ? Er1 C2 2.676(8) 3_655 ? Er1 N1 2.728(6) 3_655 ? Er1 C4 2.805(7) 3_655 ? Er1 C3 2.807(7) 3_655 ? Er1 Si2 3.360(2) . ? Er1 Si1 3.364(3) . ? Er1' N2' 2.177(5) . ? Er1' N3' 2.201(5) . ? Er1' N1' 2.356(5) . ? Er1' C1' 2.650(6) 3_766 ? Er1' N1' 2.701(5) 3_766 ? Er1' C2' 2.711(7) 3_766 ? Er1' C3' 2.786(7) 3_766 ? Er1' C4' 2.792(6) 3_766 ? Er1' Si2' 3.351(2) . ? Er1' Si1' 3.387(2) . ? Er1' Er1' 3.9587(8) 3_766 ? N1 Er1 2.728(6) 3_655 ? N3 Si1 1.702(7) . ? N3 Si2 1.712(6) . ? N1' Er1' 2.701(5) 3_766 ? N3' Si1' 1.712(6) . ? N3' Si2' 1.721(6) . ? 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 C2 C1 N1 110.4(8) . . ? C2 C1 Er1 76.5(5) . 3_655 ? N1 C1 Er1 78.5(4) . 3_655 ? C2 C1 H1 124.8 . . ? N1 C1 H1 124.8 . . ? Er1 C1 H1 112.3 3_655 . ? C1 C2 C3 107.7(7) . . ? C1 C2 Er1 73.8(5) . 3_655 ? C3 C2 Er1 80.4(5) . 3_655 ? C1 C2 H2 126.2 . . ? C3 C2 H2 126.2 . . ? Er1 C2 H2 112.2 3_655 . ? C4 C3 C2 106.6(7) . . ? C4 C3 Er1 75.8(4) . 3_655 ? C2 C3 Er1 70.0(4) . 3_655 ? C4 C3 H3 126.7 . . ? C2 C3 H3 126.7 . . ? Er1 C3 H3 119.4 3_655 . ? C3 C4 N1 110.2(7) . . ? C3 C4 C5 129.8(7) . . ? N1 C4 C5 119.2(6) . . ? C3 C4 Er1 75.9(4) . 3_655 ? N1 C4 Er1 72.3(4) . 3_655 ? C5 C4 Er1 126.0(6) . 3_655 ? N2 C5 C4 113.7(6) . . ? N2 C5 H5A 108.8 . . ? C4 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? C4 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C11 C6 C7 121.9(8) . . ? C11 C6 N2 118.9(8) . . ? C7 C6 N2 119.2(8) . . ? C8 C7 C6 116.7(10) . . ? C8 C7 C12 119.5(10) . . ? C6 C7 C12 123.7(8) . . ? C9 C8 C7 122.4(12) . . ? C9 C8 H8 118.8 . . ? C7 C8 H8 118.8 . . ? C8 C9 C10 119.9(10) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 C11 122.3(11) . . ? C9 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C6 C11 C10 116.7(10) . . ? C6 C11 C15 122.6(8) . . ? C10 C11 C15 120.7(10) . . ? C7 C12 C13 113.4(9) . . ? C7 C12 C14 110.4(10) . . ? C13 C12 C14 111.2(10) . . ? C7 C12 H12 107.1 . . ? C13 C12 H12 107.1 . . ? C14 C12 H12 107.1 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C11 112.8(9) . . ? C16 C15 C17 107.1(10) . . ? C11 C15 C17 112.3(10) . . ? C16 C15 H15 108.2 . . ? C11 C15 H15 108.2 . . ? C17 C15 H15 108.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C2' C1' N1' 111.2(6) . . ? C2' C1' Er1' 77.8(4) . 3_766 ? N1' C1' Er1' 77.2(3) . 3_766 ? C2' C1' H1' 124.4 . . ? N1' C1' H1' 124.4 . . ? Er1' C1' H1' 112.6 3_766 . ? C1' C2' C3' 107.0(6) . . ? C1' C2' Er1' 72.8(4) . 3_766 ? C3' C2' Er1' 78.0(4) . 3_766 ? C1' C2' H2' 126.5 . . ? C3' C2' H2' 126.5 . . ? Er1' C2' H2' 115.0 3_766 . ? C4' C3' C2' 106.0(6) . . ? C4' C3' Er1' 75.8(4) . 3_766 ? C2' C3' Er1' 72.2(4) . 3_766 ? C4' C3' H3' 127.0 . . ? C2' C3' H3' 127.0 . . ? Er1' C3' H3' 117.3 3_766 . ? N1' C4' C3' 109.8(6) . . ? N1' C4' C5' 120.7(5) . . ? C3' C4' C5' 128.7(6) . . ? N1' C4' Er1' 71.8(3) . 3_766 ? C3' C4' Er1' 75.2(4) . 3_766 ? C5' C4' Er1' 126.9(4) . 3_766 ? N2' C5' C4' 111.6(5) . . ? N2' C5' H5'1 109.3 . . ? C4' C5' H5'1 109.3 . . ? N2' C5' H5'2 109.3 . . ? C4' C5' H5'2 109.3 . . ? H5'1 C5' H5'2 108.0 . . ? C7' C6' C11' 120.1(6) . . ? C7' C6' N2' 120.7(6) . . ? C11' C6' N2' 119.1(6) . . ? C8' C7' C6' 118.0(7) . . ? C8' C7' C12' 119.5(7) . . ? C6' C7' C12' 122.5(6) . . ? C9' C8' C7' 123.3(7) . . ? C9' C8' H8' 118.3 . . ? C7' C8' H8' 118.3 . . ? C8' C9' C10' 118.4(7) . . ? C8' C9' H9' 120.8 . . ? C10' C9' H9' 120.8 . . ? C9' C10' C11' 121.9(7) . . ? C9' C10' H10' 119.1 . . ? C11' C10' H10' 119.1 . . ? C10' C11' C6' 118.1(7) . . ? C10' C11' C15' 119.0(7) . . ? C6' C11' C15' 122.9(6) . . ? C7' C12' C14' 112.3(6) . . ? C7' C12' C13' 111.3(6) . . ? C14' C12' C13' 111.0(6) . . ? C7' C12' H12' 107.3 . . ? C14' C12' H12' 107.3 . . ? C13' C12' H12' 107.3 . . ? C12' C13' H13D 109.5 . . ? C12' C13' H13E 109.5 . . ? H13D C13' H13E 109.5 . . ? C12' C13' H13F 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? C12' C14' H14D 109.5 . . ? C12' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C12' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? C11' C15' C17' 112.6(7) . . ? C11' C15' C16' 111.1(6) . . ? C17' C15' C16' 109.6(7) . . ? C11' C15' H15' 107.8 . . ? C17' C15' H15' 107.8 . . ? C16' C15' H15' 107.8 . . ? C15' C16' H16D 109.5 . . ? C15' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C15' C17' H17D 109.5 . . ? C15' C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? C15' C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? Si1' C18' H18D 109.5 . . ? Si1' C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? Si1' C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? Si1' C19' H19D 109.5 . . ? Si1' C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? Si1' C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? Si1' C20' H20D 109.5 . . ? Si1' C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? Si1' C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? Si2' C21' H21D 109.5 . . ? Si2' C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? Si2' C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? Si2' C22' H22D 109.5 . . ? Si2' C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? Si2' C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? Si2' C23' H23D 109.5 . . ? Si2' C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? Si2' C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? N2 Er1 N3 117.7(2) . . ? N2 Er1 N1 75.3(2) . . ? N3 Er1 N1 125.1(2) . . ? N2 Er1 C1 89.4(2) . 3_655 ? N3 Er1 C1 131.4(2) . 3_655 ? N1 Er1 C1 99.3(2) . 3_655 ? N2 Er1 C2 109.6(3) . 3_655 ? N3 Er1 C2 101.9(3) . 3_655 ? N1 Er1 C2 124.6(2) . 3_655 ? C1 Er1 C2 29.7(2) 3_655 3_655 ? N2 Er1 N1 100.0(2) . 3_655 ? N3 Er1 N1 139.95(19) . 3_655 ? N1 Er1 N1 75.2(2) . 3_655 ? C1 Er1 N1 29.9(2) 3_655 3_655 ? C2 Er1 N1 49.4(2) 3_655 3_655 ? N2 Er1 C4 129.2(2) . 3_655 ? N3 Er1 C4 111.9(2) . 3_655 ? N1 Er1 C4 85.2(2) . 3_655 ? C1 Er1 C4 47.8(2) 3_655 3_655 ? C2 Er1 C4 47.9(2) 3_655 3_655 ? N1 Er1 C4 29.3(2) 3_655 3_655 ? N2 Er1 C3 137.1(3) . 3_655 ? N3 Er1 C3 92.2(2) . 3_655 ? N1 Er1 C3 113.4(2) . 3_655 ? C1 Er1 C3 48.3(3) 3_655 3_655 ? C2 Er1 C3 29.6(3) 3_655 3_655 ? N1 Er1 C3 48.5(2) 3_655 3_655 ? C4 Er1 C3 28.3(2) 3_655 3_655 ? N2 Er1 Si2 105.38(16) . . ? N3 Er1 Si2 26.94(17) . . ? N1 Er1 Si2 149.24(16) . . ? C1 Er1 Si2 111.41(18) 3_655 . ? C2 Er1 Si2 84.79(19) 3_655 . ? N1 Er1 Si2 133.10(12) 3_655 . ? C4 Er1 Si2 114.36(15) 3_655 . ? C3 Er1 Si2 87.49(16) 3_655 . ? N2 Er1 Si1 127.89(17) . . ? N3 Er1 Si1 26.56(17) . . ? N1 Er1 Si1 101.23(16) . . ? C1 Er1 Si1 140.88(19) 3_655 . ? C2 Er1 Si1 113.8(2) 3_655 . ? N1 Er1 Si1 130.02(14) 3_655 . ? C4 Er1 Si1 101.45(18) 3_655 . ? C3 Er1 Si1 92.8(2) 3_655 . ? Si2 Er1 Si1 53.36(6) . . ? N2' Er1' N3' 117.9(2) . . ? N2' Er1' N1' 74.73(17) . . ? N3' Er1' N1' 122.51(19) . . ? N2' Er1' C1' 89.2(2) . 3_766 ? N3' Er1' C1' 132.6(2) . 3_766 ? N1' Er1' C1' 100.94(18) . 3_766 ? N2' Er1' N1' 99.78(17) . 3_766 ? N3' Er1' N1' 140.32(19) . 3_766 ? N1' Er1' N1' 77.15(17) . 3_766 ? C1' Er1' N1' 29.73(17) 3_766 3_766 ? N2' Er1' C2' 108.7(2) . 3_766 ? N3' Er1' C2' 103.3(2) . 3_766 ? N1' Er1' C2' 126.42(19) . 3_766 ? C1' Er1' C2' 29.4(2) 3_766 3_766 ? N1' Er1' C2' 49.30(18) 3_766 3_766 ? N2' Er1' C3' 136.8(2) . 3_766 ? N3' Er1' C3' 92.4(2) . 3_766 ? N1' Er1' C3' 115.74(18) . 3_766 ? C1' Er1' C3' 48.4(2) 3_766 3_766 ? N1' Er1' C3' 48.95(18) 3_766 3_766 ? C2' Er1' C3' 29.8(2) 3_766 3_766 ? N2' Er1' C4' 128.89(18) . 3_766 ? N3' Er1' C4' 112.23(19) . 3_766 ? N1' Er1' C4' 86.91(17) . 3_766 ? C1' Er1' C4' 47.60(19) 3_766 3_766 ? N1' Er1' C4' 29.12(16) 3_766 3_766 ? C2' Er1' C4' 48.15(19) 3_766 3_766 ? C3' Er1' C4' 28.99(18) 3_766 3_766 ? N2' Er1' Si2' 107.67(13) . . ? N3' Er1' Si2' 27.26(15) . . ? N1' Er1' Si2' 147.89(13) . . ? C1' Er1' Si2' 111.04(14) 3_766 . ? N1' Er1' Si2' 131.69(11) 3_766 . ? C2' Er1' Si2' 84.00(15) 3_766 . ? C3' Er1' Si2' 85.03(14) 3_766 . ? C4' Er1' Si2' 112.39(13) 3_766 . ? N2' Er1' Si1' 126.29(14) . . ? N3' Er1' Si1' 26.15(15) . . ? N1' Er1' Si1' 98.71(13) . . ? C1' Er1' Si1' 143.05(16) 3_766 . ? N1' Er1' Si1' 131.34(11) 3_766 . ? C2' Er1' Si1' 116.49(16) 3_766 . ? C3' Er1' Si1' 94.78(16) 3_766 . ? C4' Er1' Si1' 103.14(13) 3_766 . ? Si2' Er1' Si1' 53.19(5) . . ? N2' Er1' Er1' 87.66(13) . 3_766 ? N3' Er1' Er1' 147.66(15) . 3_766 ? N1' Er1' Er1' 41.69(12) . 3_766 ? C1' Er1' Er1' 61.35(13) 3_766 3_766 ? N1' Er1' Er1' 35.46(11) 3_766 3_766 ? C2' Er1' Er1' 84.75(15) 3_766 3_766 ? C3' Er1' Er1' 79.07(14) 3_766 3_766 ? C4' Er1' Er1' 51.10(12) 3_766 3_766 ? Si2' Er1' Er1' 163.28(4) . 3_766 ? Si1' Er1' Er1' 122.73(4) . 3_766 ? C1 N1 C4 105.1(6) . . ? C1 N1 Er1 144.1(5) . . ? C4 N1 Er1 109.1(5) . . ? C1 N1 Er1 71.7(4) . 3_655 ? C4 N1 Er1 78.4(4) . 3_655 ? Er1 N1 Er1 104.8(2) . 3_655 ? C6 N2 C5 109.2(6) . . ? C6 N2 Er1 134.9(5) . . ? C5 N2 Er1 115.7(4) . . ? Si1 N3 Si2 124.3(4) . . ? Si1 N3 Er1 117.9(3) . . ? Si2 N3 Er1 117.2(4) . . ? C1' N1' C4' 105.9(5) . . ? C1' N1' Er1' 143.4(4) . . ? C4' N1' Er1' 109.0(4) . . ? C1' N1' Er1' 73.1(3) . 3_766 ? C4' N1' Er1' 79.1(3) . 3_766 ? Er1' N1' Er1' 102.85(17) . 3_766 ? C6' N2' C5' 111.6(5) . . ? C6' N2' Er1' 130.6(4) . . ? C5' N2' Er1' 117.8(4) . . ? Si1' N3' Si2' 123.0(3) . . ? Si1' N3' Er1' 119.4(3) . . ? Si2' N3' Er1' 116.9(3) . . ? N3 Si1 C19 114.4(4) . . ? N3 Si1 C18 114.3(5) . . ? C19 Si1 C18 106.7(6) . . ? N3 Si1 C20 107.2(4) . . ? C19 Si1 C20 108.3(6) . . ? C18 Si1 C20 105.5(6) . . ? N3 Si1 Er1 35.5(2) . . ? C19 Si1 Er1 129.9(4) . . ? C18 Si1 Er1 121.9(5) . . ? C20 Si1 Er1 71.8(4) . . ? N3 Si2 C23 108.4(4) . . ? N3 Si2 C21 113.8(4) . . ? C23 Si2 C21 109.0(5) . . ? N3 Si2 C22 112.7(4) . . ? C23 Si2 C22 106.4(5) . . ? C21 Si2 C22 106.3(5) . . ? N3 Si2 Er1 35.8(2) . . ? C23 Si2 Er1 74.8(3) . . ? C21 Si2 Er1 138.9(3) . . ? C22 Si2 Er1 111.7(3) . . ? N3' Si1' C20' 113.2(3) . . ? N3' Si1' C19' 114.3(4) . . ? C20' Si1' C19' 106.6(4) . . ? N3' Si1' C18' 108.1(4) . . ? C20' Si1' C18' 106.8(4) . . ? C19' Si1' C18' 107.5(4) . . ? N3' Si1' Er1' 34.50(17) . . ? C20' Si1' Er1' 117.1(3) . . ? C19' Si1' Er1' 133.8(3) . . ? C18' Si1' Er1' 74.5(3) . . ? N3' Si2' C22' 112.9(3) . . ? N3' Si2' C23' 109.0(3) . . ? C22' Si2' C23' 107.4(4) . . ? N3' Si2' C21' 111.6(3) . . ? C22' Si2' C21' 109.1(4) . . ? C23' Si2' C21' 106.6(4) . . ? N3' Si2' Er1' 35.87(19) . . ? C22' Si2' Er1' 139.1(3) . . ? C23' Si2' Er1' 76.4(3) . . ? C21' Si2' Er1' 108.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 2.0(10) . . . . ? Er1 C1 C2 C3 74.1(6) 3_655 . . . ? N1 C1 C2 Er1 -72.0(5) . . . 3_655 ? C1 C2 C3 C4 -1.9(10) . . . . ? Er1 C2 C3 C4 67.6(6) 3_655 . . . ? C1 C2 C3 Er1 -69.5(6) . . . 3_655 ? C2 C3 C4 N1 1.1(9) . . . . ? Er1 C3 C4 N1 64.8(5) 3_655 . . . ? C2 C3 C4 C5 170.9(9) . . . . ? Er1 C3 C4 C5 -125.4(10) 3_655 . . . ? C2 C3 C4 Er1 -63.7(6) . . . 3_655 ? C3 C4 C5 N2 -171.7(8) . . . . ? N1 C4 C5 N2 -2.7(11) . . . . ? Er1 C4 C5 N2 85.9(8) 3_655 . . . ? C11 C6 C7 C8 -1.2(12) . . . . ? N2 C6 C7 C8 178.5(7) . . . . ? C11 C6 C7 C12 175.8(8) . . . . ? N2 C6 C7 C12 -4.5(12) . . . . ? C6 C7 C8 C9 0.5(15) . . . . ? C12 C7 C8 C9 -176.6(10) . . . . ? C7 C8 C9 C10 -0.8(18) . . . . ? C8 C9 C10 C11 1.8(18) . . . . ? C7 C6 C11 C10 2.0(12) . . . . ? N2 C6 C11 C10 -177.7(7) . . . . ? C7 C6 C11 C15 -177.0(8) . . . . ? N2 C6 C11 C15 3.3(11) . . . . ? C9 C10 C11 C6 -2.3(15) . . . . ? C9 C10 C11 C15 176.7(10) . . . . ? C8 C7 C12 C13 62.9(12) . . . . ? C6 C7 C12 C13 -114.0(10) . . . . ? C8 C7 C12 C14 -62.7(12) . . . . ? C6 C7 C12 C14 120.4(10) . . . . ? C6 C11 C15 C16 110.6(11) . . . . ? C10 C11 C15 C16 -68.4(13) . . . . ? C6 C11 C15 C17 -128.3(10) . . . . ? C10 C11 C15 C17 52.8(12) . . . . ? N1' C1' C2' C3' 0.4(8) . . . . ? Er1' C1' C2' C3' 71.2(5) 3_766 . . . ? N1' C1' C2' Er1' -70.8(4) . . . 3_766 ? C1' C2' C3' C4' 1.2(8) . . . . ? Er1' C2' C3' C4' 68.8(5) 3_766 . . . ? C1' C2' C3' Er1' -67.7(5) . . . 3_766 ? C2' C3' C4' N1' -2.3(8) . . . . ? Er1' C3' C4' N1' 64.0(4) 3_766 . . . ? C2' C3' C4' C5' 167.8(7) . . . . ? Er1' C3' C4' C5' -125.8(7) 3_766 . . . ? C2' C3' C4' Er1' -66.3(5) . . . 3_766 ? N1' C4' C5' N2' -8.2(9) . . . . ? C3' C4' C5' N2' -177.4(6) . . . . ? Er1' C4' C5' N2' 81.3(6) 3_766 . . . ? C11' C6' C7' C8' -4.9(10) . . . . ? N2' C6' C7' C8' 171.7(6) . . . . ? C11' C6' C7' C12' 174.5(6) . . . . ? N2' C6' C7' C12' -8.9(9) . . . . ? C6' C7' C8' C9' 2.1(11) . . . . ? C12' C7' C8' C9' -177.3(7) . . . . ? C7' C8' C9' C10' 0.2(12) . . . . ? C8' C9' C10' C11' 0.3(12) . . . . ? C9' C10' C11' C6' -3.0(11) . . . . ? C9' C10' C11' C15' 174.3(7) . . . . ? C7' C6' C11' C10' 5.3(10) . . . . ? N2' C6' C11' C10' -171.3(6) . . . . ? C7' C6' C11' C15' -171.9(6) . . . . ? N2' C6' C11' C15' 11.4(9) . . . . ? C8' C7' C12' C14' -61.7(9) . . . . ? C6' C7' C12' C14' 118.9(7) . . . . ? C8' C7' C12' C13' 63.4(8) . . . . ? C6' C7' C12' C13' -116.0(7) . . . . ? C10' C11' C15' C17' 55.0(9) . . . . ? C6' C11' C15' C17' -127.8(8) . . . . ? C10' C11' C15' C16' -68.4(9) . . . . ? C6' C11' C15' C16' 108.9(8) . . . . ? C2 C1 N1 C4 -1.3(9) . . . . ? Er1 C1 N1 C4 -72.0(5) 3_655 . . . ? C2 C1 N1 Er1 160.7(7) . . . . ? Er1 C1 N1 Er1 90.0(8) 3_655 . . . ? C2 C1 N1 Er1 70.7(6) . . . 3_655 ? C3 C4 N1 C1 0.1(9) . . . . ? C5 C4 N1 C1 -170.9(7) . . . . ? Er1 C4 N1 C1 67.2(5) 3_655 . . . ? C3 C4 N1 Er1 -168.9(5) . . . . ? C5 C4 N1 Er1 20.1(9) . . . . ? Er1 C4 N1 Er1 -101.8(3) 3_655 . . . ? C3 C4 N1 Er1 -67.1(6) . . . 3_655 ? C5 C4 N1 Er1 121.9(7) . . . 3_655 ? N2 Er1 N1 C1 176.3(9) . . . . ? N3 Er1 N1 C1 62.5(9) . . . . ? C1 Er1 N1 C1 -96.8(9) 3_655 . . . ? C2 Er1 N1 C1 -79.8(9) 3_655 . . . ? N1 Er1 N1 C1 -79.0(8) 3_655 . . . ? C4 Er1 N1 C1 -51.0(9) 3_655 . . . ? C3 Er1 N1 C1 -48.4(9) 3_655 . . . ? Si2 Er1 N1 C1 80.9(9) . . . . ? Si1 Er1 N1 C1 49.7(9) . . . . ? N2 Er1 N1 C4 -22.1(5) . . . . ? N3 Er1 N1 C4 -135.9(5) . . . . ? C1 Er1 N1 C4 64.8(5) 3_655 . . . ? C2 Er1 N1 C4 81.8(5) 3_655 . . . ? N1 Er1 N1 C4 82.6(5) 3_655 . . . ? C4 Er1 N1 C4 110.6(4) 3_655 . . . ? C3 Er1 N1 C4 113.2(5) 3_655 . . . ? Si2 Er1 N1 C4 -117.5(5) . . . . ? Si1 Er1 N1 C4 -148.7(4) . . . . ? N2 Er1 N1 Er1 -104.7(3) . . . 3_655 ? N3 Er1 N1 Er1 141.5(2) . . . 3_655 ? C1 Er1 N1 Er1 -17.8(3) 3_655 . . 3_655 ? C2 Er1 N1 Er1 -0.8(4) 3_655 . . 3_655 ? N1 Er1 N1 Er1 0.0 3_655 . . 3_655 ? C4 Er1 N1 Er1 28.0(2) 3_655 . . 3_655 ? C3 Er1 N1 Er1 30.6(3) 3_655 . . 3_655 ? Si2 Er1 N1 Er1 159.87(12) . . . 3_655 ? Si1 Er1 N1 Er1 128.73(17) . . . 3_655 ? C11 C6 N2 C5 -95.5(8) . . . . ? C7 C6 N2 C5 84.8(9) . . . . ? C11 C6 N2 Er1 79.9(9) . . . . ? C7 C6 N2 Er1 -99.8(8) . . . . ? C4 C5 N2 C6 157.7(7) . . . . ? C4 C5 N2 Er1 -18.7(9) . . . . ? N3 Er1 N2 C6 -31.0(8) . . . . ? N1 Er1 N2 C6 -153.3(8) . . . . ? C1 Er1 N2 C6 106.9(8) 3_655 . . . ? C2 Er1 N2 C6 84.7(8) 3_655 . . . ? N1 Er1 N2 C6 135.0(7) 3_655 . . . ? C4 Er1 N2 C6 135.8(7) 3_655 . . . ? C3 Er1 N2 C6 98.1(8) 3_655 . . . ? Si2 Er1 N2 C6 -5.2(8) . . . . ? Si1 Er1 N2 C6 -60.4(8) . . . . ? N3 Er1 N2 C5 144.2(5) . . . . ? N1 Er1 N2 C5 21.9(6) . . . . ? C1 Er1 N2 C5 -77.9(6) 3_655 . . . ? C2 Er1 N2 C5 -100.1(6) 3_655 . . . ? N1 Er1 N2 C5 -49.8(6) 3_655 . . . ? C4 Er1 N2 C5 -49.0(7) 3_655 . . . ? C3 Er1 N2 C5 -86.7(6) 3_655 . . . ? Si2 Er1 N2 C5 170.0(5) . . . . ? Si1 Er1 N2 C5 114.8(5) . . . . ? N2 Er1 N3 Si1 -120.0(3) . . . . ? N1 Er1 N3 Si1 -29.0(4) . . . . ? C1 Er1 N3 Si1 123.3(4) 3_655 . . . ? C2 Er1 N3 Si1 120.1(4) 3_655 . . . ? N1 Er1 N3 Si1 81.7(5) 3_655 . . . ? C4 Er1 N3 Si1 70.9(4) 3_655 . . . ? C3 Er1 N3 Si1 91.9(4) 3_655 . . . ? Si2 Er1 N3 Si1 171.9(6) . . . . ? N2 Er1 N3 Si2 68.1(4) . . . . ? N1 Er1 N3 Si2 159.2(3) . . . . ? C1 Er1 N3 Si2 -48.6(5) 3_655 . . . ? C2 Er1 N3 Si2 -51.8(4) 3_655 . . . ? N1 Er1 N3 Si2 -90.2(4) 3_655 . . . ? C4 Er1 N3 Si2 -100.9(3) 3_655 . . . ? C3 Er1 N3 Si2 -80.0(3) 3_655 . . . ? Si1 Er1 N3 Si2 -171.9(6) . . . . ? C2' C1' N1' C4' -1.8(7) . . . . ? Er1' C1' N1' C4' -73.1(4) 3_766 . . . ? C2' C1' N1' Er1' 160.1(5) . . . . ? Er1' C1' N1' Er1' 88.9(6) 3_766 . . . ? C2' C1' N1' Er1' 71.2(5) . . . 3_766 ? C3' C4' N1' C1' 2.6(7) . . . . ? C5' C4' N1' C1' -168.5(6) . . . . ? Er1' C4' N1' C1' 68.8(4) 3_766 . . . ? C3' C4' N1' Er1' -166.2(5) . . . . ? C5' C4' N1' Er1' 22.7(7) . . . . ? Er1' C4' N1' Er1' -100.0(2) 3_766 . . . ? C3' C4' N1' Er1' -66.2(5) . . . 3_766 ? C5' C4' N1' Er1' 122.7(6) . . . 3_766 ? N2' Er1' N1' C1' 177.1(7) . . . . ? N3' Er1' N1' C1' 63.4(7) . . . . ? C1' Er1' N1' C1' -96.9(7) 3_766 . . . ? N1' Er1' N1' C1' -78.9(7) 3_766 . . . ? C2' Er1' N1' C1' -80.7(7) 3_766 . . . ? C3' Er1' N1' C1' -48.0(7) 3_766 . . . ? C4' Er1' N1' C1' -51.1(7) 3_766 . . . ? Si2' Er1' N1' C1' 78.0(7) . . . . ? Si1' Er1' N1' C1' 51.7(7) . . . . ? Er1' Er1' N1' C1' -78.9(7) 3_766 . . . ? N2' Er1' N1' C4' -21.3(4) . . . . ? N3' Er1' N1' C4' -135.0(4) . . . . ? C1' Er1' N1' C4' 64.8(4) 3_766 . . . ? N1' Er1' N1' C4' 82.7(4) 3_766 . . . ? C2' Er1' N1' C4' 81.0(4) 3_766 . . . ? C3' Er1' N1' C4' 113.7(4) 3_766 . . . ? C4' Er1' N1' C4' 110.5(4) 3_766 . . . ? Si2' Er1' N1' C4' -120.3(4) . . . . ? Si1' Er1' N1' C4' -146.7(4) . . . . ? Er1' Er1' N1' C4' 82.7(4) 3_766 . . . ? N2' Er1' N1' Er1' -104.0(2) . . . 3_766 ? N3' Er1' N1' Er1' 142.3(2) . . . 3_766 ? C1' Er1' N1' Er1' -18.0(2) 3_766 . . 3_766 ? N1' Er1' N1' Er1' 0.0 3_766 . . 3_766 ? C2' Er1' N1' Er1' -1.8(3) 3_766 . . 3_766 ? C3' Er1' N1' Er1' 30.9(3) 3_766 . . 3_766 ? C4' Er1' N1' Er1' 27.74(18) 3_766 . . 3_766 ? Si2' Er1' N1' Er1' 156.91(12) . . . 3_766 ? Si1' Er1' N1' Er1' 130.58(13) . . . 3_766 ? C7' C6' N2' C5' 87.5(7) . . . . ? C11' C6' N2' C5' -95.9(7) . . . . ? C7' C6' N2' Er1' -94.4(7) . . . . ? C11' C6' N2' Er1' 82.3(7) . . . . ? C4' C5' N2' C6' 165.2(5) . . . . ? C4' C5' N2' Er1' -13.2(7) . . . . ? N3' Er1' N2' C6' -40.2(6) . . . . ? N1' Er1' N2' C6' -159.3(6) . . . . ? C1' Er1' N2' C6' 99.1(5) 3_766 . . . ? N1' Er1' N2' C6' 127.0(5) 3_766 . . . ? C2' Er1' N2' C6' 76.8(6) 3_766 . . . ? C3' Er1' N2' C6' 89.2(6) 3_766 . . . ? C4' Er1' N2' C6' 127.7(5) 3_766 . . . ? Si2' Er1' N2' C6' -12.7(6) . . . . ? Si1' Er1' N2' C6' -69.6(6) . . . . ? Er1' Er1' N2' C6' 160.5(5) 3_766 . . . ? N3' Er1' N2' C5' 137.8(4) . . . . ? N1' Er1' N2' C5' 18.8(4) . . . . ? C1' Er1' N2' C5' -82.8(5) 3_766 . . . ? N1' Er1' N2' C5' -54.9(5) 3_766 . . . ? C2' Er1' N2' C5' -105.1(5) 3_766 . . . ? C3' Er1' N2' C5' -92.8(5) 3_766 . . . ? C4' Er1' N2' C5' -54.3(5) 3_766 . . . ? Si2' Er1' N2' C5' 165.3(4) . . . . ? Si1' Er1' N2' C5' 108.4(4) . . . . ? Er1' Er1' N2' C5' -21.5(4) 3_766 . . . ? N2' Er1' N3' Si1' -116.1(3) . . . . ? N1' Er1' N3' Si1' -27.0(4) . . . . ? C1' Er1' N3' Si1' 126.2(3) 3_766 . . . ? N1' Er1' N3' Si1' 83.8(4) 3_766 . . . ? C2' Er1' N3' Si1' 123.9(3) 3_766 . . . ? C3' Er1' N3' Si1' 95.9(3) 3_766 . . . ? C4' Er1' N3' Si1' 74.0(4) 3_766 . . . ? Si2' Er1' N3' Si1' 170.1(6) . . . . ? Er1' Er1' N3' Si1' 22.5(5) 3_766 . . . ? N2' Er1' N3' Si2' 73.8(4) . . . . ? N1' Er1' N3' Si2' 162.9(3) . . . . ? C1' Er1' N3' Si2' -43.9(5) 3_766 . . . ? N1' Er1' N3' Si2' -86.3(4) 3_766 . . . ? C2' Er1' N3' Si2' -46.1(4) 3_766 . . . ? C3' Er1' N3' Si2' -74.2(3) 3_766 . . . ? C4' Er1' N3' Si2' -96.0(3) 3_766 . . . ? Si1' Er1' N3' Si2' -170.1(6) . . . . ? Er1' Er1' N3' Si2' -147.52(18) 3_766 . . . ? Si2 N3 Si1 C19 46.0(7) . . . . ? Er1 N3 Si1 C19 -125.2(5) . . . . ? Si2 N3 Si1 C18 -77.3(7) . . . . ? Er1 N3 Si1 C18 111.4(6) . . . . ? Si2 N3 Si1 C20 166.1(6) . . . . ? Er1 N3 Si1 C20 -5.1(6) . . . . ? Si2 N3 Si1 Er1 171.2(7) . . . . ? N2 Er1 Si1 N3 76.2(4) . . . . ? N1 Er1 Si1 N3 156.2(4) . . . . ? C1 Er1 Si1 N3 -83.4(4) 3_655 . . . ? C2 Er1 Si1 N3 -67.7(4) 3_655 . . . ? N1 Er1 Si1 N3 -123.8(4) 3_655 . . . ? C4 Er1 Si1 N3 -116.5(4) 3_655 . . . ? C3 Er1 Si1 N3 -89.3(4) 3_655 . . . ? Si2 Er1 Si1 N3 -4.6(3) . . . . ? N2 Er1 Si1 C19 152.1(6) . . . . ? N3 Er1 Si1 C19 75.9(6) . . . . ? N1 Er1 Si1 C19 -128.0(6) . . . . ? C1 Er1 Si1 C19 -7.6(6) 3_655 . . . ? C2 Er1 Si1 C19 8.1(6) 3_655 . . . ? N1 Er1 Si1 C19 -47.9(6) 3_655 . . . ? C4 Er1 Si1 C19 -40.7(6) 3_655 . . . ? C3 Er1 Si1 C19 -13.5(6) 3_655 . . . ? Si2 Er1 Si1 C19 71.3(5) . . . . ? N2 Er1 Si1 C18 -11.7(6) . . . . ? N3 Er1 Si1 C18 -87.9(6) . . . . ? N1 Er1 Si1 C18 68.3(6) . . . . ? C1 Er1 Si1 C18 -171.3(6) 3_655 . . . ? C2 Er1 Si1 C18 -155.6(6) 3_655 . . . ? N1 Er1 Si1 C18 148.4(6) 3_655 . . . ? C4 Er1 Si1 C18 155.6(6) 3_655 . . . ? C3 Er1 Si1 C18 -177.2(6) 3_655 . . . ? Si2 Er1 Si1 C18 -92.5(5) . . . . ? N2 Er1 Si1 C20 -108.9(5) . . . . ? N3 Er1 Si1 C20 174.9(6) . . . . ? N1 Er1 Si1 C20 -29.0(5) . . . . ? C1 Er1 Si1 C20 91.4(5) 3_655 . . . ? C2 Er1 Si1 C20 107.1(5) 3_655 . . . ? N1 Er1 Si1 C20 51.1(5) 3_655 . . . ? C4 Er1 Si1 C20 58.3(5) 3_655 . . . ? C3 Er1 Si1 C20 85.5(5) 3_655 . . . ? Si2 Er1 Si1 C20 170.3(5) . . . . ? Si1 N3 Si2 C23 167.2(5) . . . . ? Er1 N3 Si2 C23 -21.5(5) . . . . ? Si1 N3 Si2 C21 45.9(6) . . . . ? Er1 N3 Si2 C21 -142.8(5) . . . . ? Si1 N3 Si2 C22 -75.3(6) . . . . ? Er1 N3 Si2 C22 96.0(4) . . . . ? Si1 N3 Si2 Er1 -171.3(6) . . . . ? N2 Er1 Si2 N3 -121.6(4) . . . . ? N1 Er1 Si2 N3 -34.7(4) . . . . ? C1 Er1 Si2 N3 142.9(4) 3_655 . . . ? C2 Er1 Si2 N3 129.5(4) 3_655 . . . ? N1 Er1 Si2 N3 118.2(4) 3_655 . . . ? C4 Er1 Si2 N3 90.8(4) 3_655 . . . ? C3 Er1 Si2 N3 99.9(4) 3_655 . . . ? Si1 Er1 Si2 N3 4.5(3) . . . . ? N2 Er1 Si2 C23 37.3(4) . . . . ? N3 Er1 Si2 C23 158.9(5) . . . . ? N1 Er1 Si2 C23 124.2(4) . . . . ? C1 Er1 Si2 C23 -58.2(4) 3_655 . . . ? C2 Er1 Si2 C23 -71.6(4) 3_655 . . . ? N1 Er1 Si2 C23 -82.9(4) 3_655 . . . ? C4 Er1 Si2 C23 -110.3(4) 3_655 . . . ? C3 Er1 Si2 C23 -101.2(4) 3_655 . . . ? Si1 Er1 Si2 C23 163.4(4) . . . . ? N2 Er1 Si2 C21 -64.3(6) . . . . ? N3 Er1 Si2 C21 57.3(7) . . . . ? N1 Er1 Si2 C21 22.6(7) . . . . ? C1 Er1 Si2 C21 -159.9(7) 3_655 . . . ? C2 Er1 Si2 C21 -173.2(6) 3_655 . . . ? N1 Er1 Si2 C21 175.5(6) 3_655 . . . ? C4 Er1 Si2 C21 148.1(6) 3_655 . . . ? C3 Er1 Si2 C21 157.2(6) 3_655 . . . ? Si1 Er1 Si2 C21 61.8(6) . . . . ? N2 Er1 Si2 C22 139.3(4) . . . . ? N3 Er1 Si2 C22 -99.1(5) . . . . ? N1 Er1 Si2 C22 -133.8(4) . . . . ? C1 Er1 Si2 C22 43.7(4) 3_655 . . . ? C2 Er1 Si2 C22 30.3(4) 3_655 . . . ? N1 Er1 Si2 C22 19.1(4) 3_655 . . . ? C4 Er1 Si2 C22 -8.4(4) 3_655 . . . ? C3 Er1 Si2 C22 0.8(4) 3_655 . . . ? Si1 Er1 Si2 C22 -94.6(4) . . . . ? Si2' N3' Si1' C20' -86.0(5) . . . . ? Er1' N3' Si1' C20' 104.6(4) . . . . ? Si2' N3' Si1' C19' 36.3(6) . . . . ? Er1' N3' Si1' C19' -133.1(4) . . . . ? Si2' N3' Si1' C18' 155.9(5) . . . . ? Er1' N3' Si1' C18' -13.5(5) . . . . ? Si2' N3' Si1' Er1' 169.4(6) . . . . ? N2' Er1' Si1' N3' 79.8(4) . . . . ? N1' Er1' Si1' N3' 157.2(4) . . . . ? C1' Er1' Si1' N3' -81.3(4) 3_766 . . . ? N1' Er1' Si1' N3' -122.3(4) 3_766 . . . ? C2' Er1' Si1' N3' -64.4(4) 3_766 . . . ? C3' Er1' Si1' N3' -85.8(4) 3_766 . . . ? C4' Er1' Si1' N3' -114.0(4) 3_766 . . . ? Si2' Er1' Si1' N3' -5.7(3) . . . . ? Er1' Er1' Si1' N3' -165.9(3) 3_766 . . . ? N2' Er1' Si1' C20' -12.3(4) . . . . ? N3' Er1' Si1' C20' -92.1(5) . . . . ? N1' Er1' Si1' C20' 65.1(3) . . . . ? C1' Er1' Si1' C20' -173.4(4) 3_766 . . . ? N1' Er1' Si1' C20' 145.6(3) 3_766 . . . ? C2' Er1' Si1' C20' -156.5(4) 3_766 . . . ? C3' Er1' Si1' C20' -177.9(3) 3_766 . . . ? C4' Er1' Si1' C20' 154.0(3) 3_766 . . . ? Si2' Er1' Si1' C20' -97.8(3) . . . . ? Er1' Er1' Si1' C20' 102.0(3) 3_766 . . . ? N2' Er1' Si1' C19' 146.9(4) . . . . ? N3' Er1' Si1' C19' 67.1(5) . . . . ? N1' Er1' Si1' C19' -135.7(4) . . . . ? C1' Er1' Si1' C19' -14.1(5) 3_766 . . . ? N1' Er1' Si1' C19' -55.2(4) 3_766 . . . ? C2' Er1' Si1' C19' 2.7(4) 3_766 . . . ? C3' Er1' Si1' C19' -18.7(4) 3_766 . . . ? C4' Er1' Si1' C19' -46.8(4) 3_766 . . . ? Si2' Er1' Si1' C19' 61.5(4) . . . . ? Er1' Er1' Si1' C19' -98.8(4) 3_766 . . . ? N2' Er1' Si1' C18' -113.5(4) . . . . ? N3' Er1' Si1' C18' 166.7(5) . . . . ? N1' Er1' Si1' C18' -36.1(4) . . . . ? C1' Er1' Si1' C18' 85.4(4) 3_766 . . . ? N1' Er1' Si1' C18' 44.4(4) 3_766 . . . ? C2' Er1' Si1' C18' 102.2(4) 3_766 . . . ? C3' Er1' Si1' C18' 80.9(4) 3_766 . . . ? C4' Er1' Si1' C18' 52.7(4) 3_766 . . . ? Si2' Er1' Si1' C18' 161.0(3) . . . . ? Er1' Er1' Si1' C18' 0.8(3) 3_766 . . . ? Si1' N3' Si2' C22' 45.5(5) . . . . ? Er1' N3' Si2' C22' -144.8(4) . . . . ? Si1' N3' Si2' C23' 164.8(4) . . . . ? Er1' N3' Si2' C23' -25.5(5) . . . . ? Si1' N3' Si2' C21' -77.7(5) . . . . ? Er1' N3' Si2' C21' 91.9(4) . . . . ? Si1' N3' Si2' Er1' -169.7(6) . . . . ? N2' Er1' Si2' N3' -117.1(4) . . . . ? N1' Er1' Si2' N3' -27.8(4) . . . . ? C1' Er1' Si2' N3' 146.9(4) 3_766 . . . ? N1' Er1' Si2' N3' 121.4(4) 3_766 . . . ? C2' Er1' Si2' N3' 135.1(4) 3_766 . . . ? C3' Er1' Si2' N3' 105.2(4) 3_766 . . . ? C4' Er1' Si2' N3' 95.4(4) 3_766 . . . ? Si1' Er1' Si2' N3' 5.4(3) . . . . ? Er1' Er1' Si2' N3' 87.2(4) 3_766 . . . ? N2' Er1' Si2' C22' -62.8(5) . . . . ? N3' Er1' Si2' C22' 54.3(6) . . . . ? N1' Er1' Si2' C22' 26.5(5) . . . . ? C1' Er1' Si2' C22' -158.9(5) 3_766 . . . ? N1' Er1' Si2' C22' 175.7(5) 3_766 . . . ? C2' Er1' Si2' C22' -170.6(5) 3_766 . . . ? C3' Er1' Si2' C22' 159.5(5) 3_766 . . . ? C4' Er1' Si2' C22' 149.6(5) 3_766 . . . ? Si1' Er1' Si2' C22' 59.7(5) . . . . ? Er1' Er1' Si2' C22' 141.4(5) 3_766 . . . ? N2' Er1' Si2' C23' 38.2(3) . . . . ? N3' Er1' Si2' C23' 155.2(5) . . . . ? N1' Er1' Si2' C23' 127.5(4) . . . . ? C1' Er1' Si2' C23' -57.9(3) 3_766 . . . ? N1' Er1' Si2' C23' -83.3(3) 3_766 . . . ? C2' Er1' Si2' C23' -69.6(3) 3_766 . . . ? C3' Er1' Si2' C23' -99.6(3) 3_766 . . . ? C4' Er1' Si2' C23' -109.4(3) 3_766 . . . ? Si1' Er1' Si2' C23' 160.7(3) . . . . ? Er1' Er1' Si2' C23' -117.6(3) 3_766 . . . ? N2' Er1' Si2' C21' 141.4(3) . . . . ? N3' Er1' Si2' C21' -101.6(5) . . . . ? N1' Er1' Si2' C21' -129.3(4) . . . . ? C1' Er1' Si2' C21' 45.3(4) 3_766 . . . ? N1' Er1' Si2' C21' 19.9(4) 3_766 . . . ? C2' Er1' Si2' C21' 33.6(3) 3_766 . . . ? C3' Er1' Si2' C21' 3.6(3) 3_766 . . . ? C4' Er1' Si2' C21' -6.2(3) 3_766 . . . ? Si1' Er1' Si2' C21' -96.1(3) . . . . ? Er1' Er1' Si2' C21' -14.4(4) 3_766 . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.175 _refine_diff_density_min -1.544 _refine_diff_density_rms 0.134