# 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_shelxl _database_code_depnum_ccdc_archive 'CCDC 900280' #TrackingRef 'CCDC 900280.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H46 La N3 Si4, 0.5(C7 H8)' _chemical_formula_sum 'C29.50 H50 La N3 Si4' _chemical_formula_weight 697.99 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.909(3) _cell_length_b 12.700(2) _cell_length_c 17.894(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.892(5) _cell_angle_gamma 90.00 _cell_volume 3822.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14364 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 1.263 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.402 _exptl_absorpt_correction_T_max 0.606 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36081 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7002 _reflns_number_gt 5801 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+7.0924P] 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 7002 _refine_ls_number_parameters 344 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1596 _refine_ls_wR_factor_gt 0.1492 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.166 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.71731(2) 0.36608(3) 0.518491(19) 0.06743(16) Uani 1 1 d . . . Si1 Si 0.53049(12) 0.22688(18) 0.49304(15) 0.0976(7) Uani 1 1 d D . . H1 H 0.515(4) 0.336(2) 0.512(4) 0.117 Uiso 1 1 d D . . Si2 Si 0.68730(14) 0.13132(19) 0.45231(14) 0.0959(7) Uani 1 1 d D A . H2 H 0.764(2) 0.184(5) 0.448(4) 0.115 Uiso 1 1 d D . . Si3 Si 0.6663(3) 0.5133(4) 0.3606(3) 0.0951(10) Uiso 0.50 1 d PD A 1 H3 H 0.583(3) 0.491(11) 0.370(10) 0.114 Uiso 0.50 1 d PD B 1 Si3' Si 0.6650(3) 0.4713(4) 0.3453(3) 0.0951(10) Uiso 0.50 1 d PD A 2 H3' H 0.590(5) 0.443(11) 0.374(9) 0.114 Uiso 0.50 1 d PD C 2 Si4 Si 0.84386(13) 0.44029(18) 0.39601(12) 0.0877(6) Uani 1 1 d D A . H4 H 0.858(4) 0.364(4) 0.457(3) 0.105 Uiso 1 1 d D . . N1 N 0.8092(3) 0.2494(4) 0.6156(3) 0.0747(14) Uani 1 1 d . A . N2 N 0.6291(3) 0.2233(4) 0.4861(3) 0.0786(15) Uani 1 1 d . A . N3 N 0.7465(3) 0.4463(5) 0.4039(3) 0.0881(17) Uani 1 1 d D A . C1 C 0.6889(4) 0.4296(5) 0.6685(3) 0.0672(15) Uani 1 1 d . A . C2 C 0.6289(4) 0.4765(6) 0.6197(4) 0.0773(18) Uani 1 1 d . A . H2A H 0.5720 0.4661 0.6230 0.093 Uiso 1 1 calc R . . C3 C 0.6603(5) 0.5542(6) 0.5749(4) 0.085(2) Uani 1 1 d . A . H3A H 0.6289 0.6072 0.5451 0.102 Uiso 1 1 calc R . . C4 C 0.7424(5) 0.5607(5) 0.5972(4) 0.0805(18) Uani 1 1 d . A . C5 C 0.8036(7) 0.6241(6) 0.5714(5) 0.106(3) Uani 1 1 d . . . H5 H 0.7921 0.6736 0.5336 0.127 Uiso 1 1 calc R A . C6 C 0.8797(7) 0.6102(8) 0.6036(7) 0.118(3) Uani 1 1 d . A . H6 H 0.9204 0.6509 0.5873 0.141 Uiso 1 1 calc R . . C7 C 0.8978(5) 0.5360(8) 0.6607(6) 0.111(3) Uani 1 1 d . . . H7 H 0.9502 0.5291 0.6816 0.134 Uiso 1 1 calc R A . C8 C 0.8414(4) 0.4740(6) 0.6862(4) 0.0846(19) Uani 1 1 d . A . H8 H 0.8553 0.4248 0.7238 0.102 Uiso 1 1 calc R . . C9 C 0.7607(4) 0.4840(5) 0.6557(4) 0.0695(16) Uani 1 1 d . A . C10 C 0.6779(4) 0.3434(5) 0.7252(4) 0.0757(17) Uani 1 1 d . . . C11 C 0.7019(4) 0.2346(5) 0.6954(4) 0.0782(18) Uani 1 1 d . A . H11A H 0.6887 0.1815 0.7311 0.094 Uiso 1 1 calc R . . H11B H 0.6692 0.2211 0.6487 0.094 Uiso 1 1 calc R . . C12 C 0.7867(4) 0.2191(5) 0.6817(4) 0.0698(16) Uani 1 1 d . . . C13 C 0.8412(5) 0.1715(6) 0.7350(4) 0.086(2) Uani 1 1 d . A . H13 H 0.8251 0.1494 0.7806 0.103 Uiso 1 1 calc R . . C14 C 0.9176(5) 0.1573(6) 0.7206(5) 0.099(2) Uani 1 1 d . . . H14 H 0.9539 0.1258 0.7562 0.119 Uiso 1 1 calc R A . C15 C 0.9408(5) 0.1892(7) 0.6541(5) 0.098(2) Uani 1 1 d . A . H15 H 0.9931 0.1802 0.6436 0.118 Uiso 1 1 calc R . . C16 C 0.8861(5) 0.2349(6) 0.6027(4) 0.089(2) Uani 1 1 d . . . H16 H 0.9021 0.2569 0.5571 0.106 Uiso 1 1 calc R A . C17 C 0.5878(5) 0.3338(7) 0.7364(5) 0.100(2) Uani 1 1 d . A . H17A H 0.5683 0.4008 0.7513 0.151 Uiso 1 1 calc R . . H17B H 0.5810 0.2825 0.7746 0.151 Uiso 1 1 calc R . . H17C H 0.5586 0.3122 0.6900 0.151 Uiso 1 1 calc R . . C18 C 0.7223(5) 0.3674(6) 0.8021(4) 0.095(2) Uani 1 1 d . A . H18A H 0.7776 0.3787 0.7968 0.143 Uiso 1 1 calc R . . H18B H 0.7169 0.3091 0.8353 0.143 Uiso 1 1 calc R . . H18C H 0.7004 0.4296 0.8226 0.143 Uiso 1 1 calc R . . C19 C 0.4670(6) 0.1968(9) 0.4046(6) 0.141(4) Uani 1 1 d . A . H19A H 0.4801 0.2439 0.3657 0.212 Uiso 1 1 calc R . . H19B H 0.4121 0.2054 0.4125 0.212 Uiso 1 1 calc R . . H19C H 0.4761 0.1255 0.3898 0.212 Uiso 1 1 calc R . . C20 C 0.4983(6) 0.1373(8) 0.5673(6) 0.134(4) Uani 1 1 d . A . H20A H 0.5145 0.0665 0.5578 0.202 Uiso 1 1 calc R . . H20B H 0.4414 0.1398 0.5666 0.202 Uiso 1 1 calc R . . H20C H 0.5223 0.1595 0.6157 0.202 Uiso 1 1 calc R . . C21 C 0.7029(7) 0.0118(9) 0.5128(6) 0.149(3) Uani 1 1 d . . . H21A H 0.7368 0.0292 0.5575 0.223 Uiso 1 1 calc R A . H21B H 0.7274 -0.0424 0.4857 0.223 Uiso 1 1 calc R . . H21C H 0.6526 -0.0127 0.5264 0.223 Uiso 1 1 calc R . . C22 C 0.6633(7) 0.0875(9) 0.3538(6) 0.149(3) Uani 1 1 d . . . H22A H 0.6165 0.0442 0.3502 0.223 Uiso 1 1 calc R A . H22B H 0.7070 0.0477 0.3383 0.223 Uiso 1 1 calc R . . H22C H 0.6539 0.1479 0.3218 0.223 Uiso 1 1 calc R . . C23 C 0.6381(13) 0.4575(17) 0.2645(10) 0.137(4) Uiso 0.50 1 d PD A 1 H23A H 0.6850 0.4494 0.2390 0.206 Uiso 0.50 1 calc PR A 1 H23B H 0.6017 0.5043 0.2365 0.206 Uiso 0.50 1 calc PR A 1 H23C H 0.6133 0.3901 0.2690 0.206 Uiso 0.50 1 calc PR A 1 C23' C 0.6519(15) 0.3929(17) 0.2575(11) 0.137(4) Uiso 0.50 1 d PD A 2 H23D H 0.7007 0.3930 0.2343 0.206 Uiso 0.50 1 calc PR A 2 H23E H 0.6104 0.4234 0.2237 0.206 Uiso 0.50 1 calc PR A 2 H23F H 0.6380 0.3219 0.2690 0.206 Uiso 0.50 1 calc PR A 2 C24 C 0.6715(15) 0.6606(12) 0.3595(14) 0.137(4) Uiso 0.50 1 d PD A 1 H24A H 0.6939 0.6855 0.4077 0.206 Uiso 0.50 1 calc PR A 1 H24B H 0.6190 0.6890 0.3485 0.206 Uiso 0.50 1 calc PR A 1 H24C H 0.7042 0.6830 0.3217 0.206 Uiso 0.50 1 calc PR A 1 C24' C 0.6601(15) 0.6182(12) 0.3311(14) 0.137(4) Uiso 0.50 1 d PD A 2 H24D H 0.6315 0.6495 0.3690 0.206 Uiso 0.50 1 calc PR A 2 H24E H 0.6334 0.6335 0.2824 0.206 Uiso 0.50 1 calc PR A 2 H24F H 0.7130 0.6464 0.3346 0.206 Uiso 0.50 1 calc PR A 2 C25 C 0.8949(6) 0.5661(7) 0.3889(6) 0.126(3) Uani 1 1 d . . . H25A H 0.8904 0.5884 0.3374 0.190 Uiso 1 1 calc R A . H25B H 0.9500 0.5582 0.4070 0.190 Uiso 1 1 calc R . . H25C H 0.8711 0.6180 0.4186 0.190 Uiso 1 1 calc R . . C26 C 0.8716(6) 0.3499(8) 0.3212(6) 0.128(3) Uani 1 1 d . . . H26A H 0.8451 0.2836 0.3253 0.193 Uiso 1 1 calc R A . H26B H 0.9281 0.3392 0.3270 0.193 Uiso 1 1 calc R . . H26C H 0.8559 0.3804 0.2729 0.193 Uiso 1 1 calc R . . C27 C 0.9556(15) -0.033(2) 0.4949(16) 0.169(4) Uiso 0.50 1 d PD . . C28 C 0.9289(16) 0.034(2) 0.4332(15) 0.169(4) Uiso 0.50 1 d PD . . C29 C 0.9873(18) 0.112(2) 0.4242(15) 0.169(4) Uiso 0.50 1 d PD . . C30 C 1.0550(16) 0.104(2) 0.4726(16) 0.169(4) Uiso 0.50 1 d PD . . C31 C 1.0845(15) 0.034(2) 0.5346(17) 0.169(4) Uiso 0.50 1 d PD . . C32 C 1.0258(15) -0.046(2) 0.5418(16) 0.169(4) Uiso 0.50 1 d PD . . C33 C 0.8959(16) -0.1248(19) 0.4942(18) 0.169(4) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0772(3) 0.0715(3) 0.0535(2) 0.00116(16) 0.00617(16) 0.00704(18) Si1 0.0721(13) 0.0887(14) 0.1269(19) -0.0120(13) -0.0140(12) -0.0017(10) Si2 0.0928(15) 0.1022(16) 0.0912(15) -0.0177(12) 0.0021(12) -0.0033(12) Si4 0.0925(14) 0.0970(15) 0.0750(13) 0.0020(11) 0.0167(11) -0.0019(11) N1 0.083(4) 0.082(4) 0.059(3) 0.001(3) 0.005(3) 0.014(3) N2 0.069(3) 0.090(4) 0.073(3) 0.005(3) -0.006(3) -0.002(3) N3 0.081(4) 0.105(4) 0.078(4) 0.012(3) 0.010(3) 0.002(3) C1 0.073(4) 0.072(4) 0.057(3) -0.003(3) 0.008(3) 0.002(3) C2 0.069(4) 0.092(5) 0.071(4) -0.007(4) 0.009(3) 0.016(3) C3 0.106(6) 0.077(5) 0.071(4) 0.006(3) 0.015(4) 0.031(4) C4 0.091(5) 0.073(4) 0.080(5) -0.006(3) 0.023(4) 0.001(4) C5 0.148(9) 0.075(5) 0.102(6) -0.009(4) 0.043(6) -0.011(5) C6 0.116(8) 0.099(7) 0.145(9) -0.025(6) 0.045(7) -0.033(6) C7 0.085(6) 0.111(7) 0.141(8) -0.027(6) 0.024(5) -0.020(5) C8 0.078(5) 0.085(5) 0.090(5) -0.018(4) 0.006(4) -0.001(4) C9 0.074(4) 0.065(4) 0.071(4) 0.000(3) 0.013(3) 0.006(3) C10 0.086(4) 0.081(4) 0.061(4) 0.002(3) 0.014(3) 0.000(3) C11 0.082(4) 0.083(5) 0.069(4) 0.001(3) 0.007(3) -0.004(4) C12 0.081(4) 0.060(4) 0.067(4) -0.004(3) 0.001(3) 0.000(3) C13 0.097(5) 0.084(5) 0.075(4) 0.015(4) 0.000(4) 0.009(4) C14 0.093(6) 0.100(6) 0.100(6) 0.019(5) -0.006(5) 0.027(4) C15 0.082(5) 0.106(6) 0.106(6) 0.013(5) 0.006(4) 0.027(4) C16 0.091(5) 0.099(5) 0.078(5) 0.005(4) 0.018(4) 0.020(4) C17 0.091(5) 0.115(6) 0.102(6) 0.003(5) 0.040(5) -0.006(4) C18 0.131(7) 0.098(5) 0.055(4) -0.005(4) 0.002(4) 0.003(5) C19 0.109(7) 0.135(8) 0.164(10) -0.001(7) -0.060(7) 0.000(6) C20 0.113(7) 0.163(10) 0.134(8) -0.026(7) 0.040(6) -0.056(6) C21 0.167(7) 0.132(6) 0.145(7) -0.022(5) 0.008(6) 0.005(5) C22 0.167(7) 0.132(6) 0.145(7) -0.022(5) 0.008(6) 0.005(5) C25 0.140(8) 0.110(7) 0.140(8) -0.009(6) 0.064(7) -0.021(6) C26 0.130(8) 0.147(9) 0.116(7) -0.039(6) 0.048(6) -0.019(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 La1 N2 2.381(5) . ? La1 N3 2.386(6) . ? La1 N1 2.660(5) . ? La1 C3 2.802(7) . ? La1 C2 2.835(6) . ? La1 C4 2.855(7) . ? La1 C1 2.890(6) . ? La1 C9 2.905(6) . ? La1 Si2 3.229(2) . ? La1 Si4 3.352(2) . ? La1 Si3' 3.407(5) . ? La1 Si3 3.424(5) . ? Si1 N2 1.686(6) . ? Si1 C19 1.859(9) . ? Si1 C20 1.873(10) . ? Si1 H1 1.459(10) . ? Si2 N2 1.680(6) . ? Si2 C22 1.854(11) . ? Si2 C21 1.867(12) . ? Si2 H2 1.461(10) . ? Si3 N3 1.716(7) . ? Si3 C24 1.874(15) . ? Si3 C23 1.875(15) . ? Si3 H3 1.460(10) . ? Si3 H3' 1.61(6) . ? Si3' N3 1.673(8) . ? Si3' C23' 1.853(15) . ? Si3' C24' 1.884(15) . ? Si3' H3 1.52(6) . ? Si3' H3' 1.461(10) . ? Si4 N3 1.669(6) . ? Si4 C25 1.827(9) . ? Si4 C26 1.859(9) . ? Si4 H4 1.450(10) . ? N1 C12 1.335(8) . ? N1 C16 1.356(8) . ? C1 C2 1.401(9) . ? C1 C9 1.436(9) . ? C1 C10 1.517(9) . ? C2 C3 1.409(10) . ? C2 H2A 0.9800 . ? C3 C4 1.408(10) . ? C3 H3A 0.9800 . ? C4 C5 1.425(11) . ? C4 C9 1.440(9) . ? C5 C6 1.366(14) . ? C5 H5 0.9300 . ? C6 C7 1.401(14) . ? C6 H6 0.9300 . ? C7 C8 1.353(11) . ? C7 H7 0.9300 . ? C8 C9 1.422(9) . ? C8 H8 0.9300 . ? C10 C18 1.530(9) . ? C10 C11 1.550(9) . ? C10 C17 1.562(10) . ? C11 C12 1.492(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.395(9) . ? C13 C14 1.355(11) . ? C13 H13 0.9300 . ? C14 C15 1.352(11) . ? C14 H14 0.9300 . ? C15 C16 1.365(10) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C23' H23D 0.9600 . ? C23' H23E 0.9600 . ? C23' H23F 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C24' H24D 0.9600 . ? C24' H24E 0.9600 . ? C24' H24F 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C31 0.82(3) 3_756 ? C27 C30 1.10(3) 3_756 ? C27 C32 1.25(3) 3_756 ? C27 C32 1.391(17) . ? C27 C28 1.428(18) . ? C27 C33 1.546(17) . ? C27 C27 1.71(5) 3_756 ? C27 C29 1.94(3) 3_756 ? C28 C32 0.86(3) 3_756 ? C28 C31 1.08(3) 3_756 ? C28 C29 1.419(18) . ? C29 C32 1.08(3) 3_756 ? C29 C30 1.367(18) . ? C29 C27 1.94(3) 3_756 ? C30 C33 1.01(3) 3_756 ? C30 C27 1.10(3) 3_756 ? C30 C31 1.465(18) . ? C30 C32 1.55(3) 3_756 ? C31 C27 0.82(3) 3_756 ? C31 C28 1.08(3) 3_756 ? C31 C33 1.32(3) 3_756 ? C31 C32 1.435(17) . ? C32 C28 0.86(3) 3_756 ? C32 C29 1.08(3) 3_756 ? C32 C27 1.25(3) 3_756 ? C32 C30 1.55(3) 3_756 ? C32 C32 2.02(5) 3_756 ? C33 C30 1.01(3) 3_756 ? C33 C31 1.32(3) 3_756 ? 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 N2 La1 N3 107.2(2) . . ? N2 La1 N1 92.53(18) . . ? N3 La1 N1 129.88(18) . . ? N2 La1 C3 120.4(2) . . ? N3 La1 C3 93.1(2) . . ? N1 La1 C3 116.03(19) . . ? N2 La1 C2 100.0(2) . . ? N3 La1 C2 120.5(2) . . ? N1 La1 C2 99.71(18) . . ? C3 La1 C2 28.9(2) . . ? N2 La1 C4 146.8(2) . . ? N3 La1 C4 91.2(2) . . ? N1 La1 C4 96.45(19) . . ? C3 La1 C4 28.8(2) . . ? C2 La1 C4 47.0(2) . . ? N2 La1 C1 106.20(19) . . ? N3 La1 C1 138.4(2) . . ? N1 La1 C1 71.95(17) . . ? C3 La1 C1 48.04(19) . . ? C2 La1 C1 28.30(17) . . ? C4 La1 C1 47.96(19) . . ? N2 La1 C9 134.10(18) . . ? N3 La1 C9 116.7(2) . . ? N1 La1 C9 69.81(17) . . ? C3 La1 C9 47.37(19) . . ? C2 La1 C9 46.30(18) . . ? C4 La1 C9 28.93(18) . . ? C1 La1 C9 28.69(17) . . ? N2 La1 Si2 30.31(14) . . ? N3 La1 Si2 96.76(16) . . ? N1 La1 Si2 77.57(13) . . ? C3 La1 Si2 150.71(18) . . ? C2 La1 Si2 128.15(16) . . ? C4 La1 Si2 171.96(15) . . ? C1 La1 Si2 124.31(13) . . ? C9 La1 Si2 143.37(13) . . ? N2 La1 Si4 118.74(14) . . ? N3 La1 Si4 27.86(14) . . ? N1 La1 Si4 102.40(13) . . ? C3 La1 Si4 105.20(16) . . ? C2 La1 Si4 133.84(16) . . ? C4 La1 Si4 90.38(15) . . ? C1 La1 Si4 134.99(13) . . ? C9 La1 Si4 106.54(13) . . ? Si2 La1 Si4 96.12(6) . . ? N2 La1 Si3' 88.82(16) . . ? N3 La1 Si3' 26.89(16) . . ? N1 La1 Si3' 153.19(15) . . ? C3 La1 Si3' 85.79(17) . . ? C2 La1 Si3' 106.42(16) . . ? C4 La1 Si3' 96.95(17) . . ? C1 La1 Si3' 133.08(15) . . ? C9 La1 Si3' 125.88(16) . . ? Si2 La1 Si3' 90.69(10) . . ? Si4 La1 Si3' 54.45(10) . . ? N2 La1 Si3 96.69(16) . . ? N3 La1 Si3 27.68(16) . . ? N1 La1 Si3 157.55(15) . . ? C3 La1 Si3 76.40(17) . . ? C2 La1 Si3 98.77(17) . . ? C4 La1 Si3 86.94(17) . . ? C1 La1 Si3 124.20(15) . . ? C9 La1 Si3 115.87(16) . . ? Si2 La1 Si3 100.65(10) . . ? Si4 La1 Si3 55.29(10) . . ? Si3' La1 Si3 10.07(11) . . ? N2 Si1 C19 114.9(4) . . ? N2 Si1 C20 113.5(4) . . ? C19 Si1 C20 107.2(5) . . ? N2 Si1 H1 104(3) . . ? C19 Si1 H1 107(3) . . ? C20 Si1 H1 110(3) . . ? N2 Si2 C22 118.2(4) . . ? N2 Si2 C21 114.2(4) . . ? C22 Si2 C21 108.2(5) . . ? N2 Si2 La1 45.67(19) . . ? C22 Si2 La1 129.6(4) . . ? C21 Si2 La1 122.0(3) . . ? N2 Si2 H2 105(3) . . ? C22 Si2 H2 101(3) . . ? C21 Si2 H2 109(3) . . ? La1 Si2 H2 60(3) . . ? N3 Si3 C24 117.6(9) . . ? N3 Si3 C23 109.9(8) . . ? C24 Si3 C23 112.1(11) . . ? N3 Si3 La1 40.2(2) . . ? C24 Si3 La1 123.1(8) . . ? C23 Si3 La1 124.7(7) . . ? N3 Si3 H3 125(6) . . ? C24 Si3 H3 104(6) . . ? C23 Si3 H3 83(7) . . ? La1 Si3 H3 88(7) . . ? N3 Si3 H3' 105(5) . . ? C24 Si3 H3' 127(5) . . ? C23 Si3 H3' 78(6) . . ? La1 Si3 H3' 73(6) . . ? H3 Si3 H3' 23(8) . . ? N3 Si3' C23' 116.6(8) . . ? N3 Si3' C24' 107.1(8) . . ? C23' Si3' C24' 114.7(11) . . ? N3 Si3' La1 40.2(2) . . ? C23' Si3' La1 123.9(8) . . ? C24' Si3' La1 121.0(8) . . ? N3 Si3' H3 124(7) . . ? C23' Si3' H3 108(6) . . ? C24' Si3' H3 81(5) . . ? La1 Si3' H3 88(7) . . ? N3 Si3' H3' 115(7) . . ? C23' Si3' H3' 98(7) . . ? C24' Si3' H3' 106(6) . . ? La1 Si3' H3' 74(7) . . ? H3 Si3' H3' 24(8) . . ? N3 Si4 C25 116.3(4) . . ? N3 Si4 C26 114.4(4) . . ? C25 Si4 C26 109.5(4) . . ? N3 Si4 La1 41.9(2) . . ? C25 Si4 La1 129.0(3) . . ? C26 Si4 La1 121.5(3) . . ? N3 Si4 H4 93(3) . . ? C25 Si4 H4 126(3) . . ? C26 Si4 H4 95(3) . . ? La1 Si4 H4 52(3) . . ? C12 N1 C16 118.5(6) . . ? C12 N1 La1 122.6(4) . . ? C16 N1 La1 118.1(4) . . ? Si2 N2 Si1 131.7(4) . . ? Si2 N2 La1 104.0(3) . . ? Si1 N2 La1 124.2(3) . . ? Si4 N3 Si3' 135.4(4) . . ? Si4 N3 Si3 136.5(4) . . ? Si3' N3 Si3 20.3(2) . . ? Si4 N3 La1 110.2(3) . . ? Si3' N3 La1 112.9(3) . . ? Si3 N3 La1 112.1(3) . . ? C2 C1 C9 105.4(6) . . ? C2 C1 C10 126.4(6) . . ? C9 C1 C10 128.1(6) . . ? C2 C1 La1 73.7(4) . . ? C9 C1 La1 76.2(3) . . ? C10 C1 La1 117.6(4) . . ? C1 C2 C3 111.2(6) . . ? C1 C2 La1 78.0(4) . . ? C3 C2 La1 74.3(4) . . ? C1 C2 H2A 123.9 . . ? C3 C2 H2A 123.9 . . ? La1 C2 H2A 123.9 . . ? C4 C3 C2 107.3(6) . . ? C4 C3 La1 77.7(4) . . ? C2 C3 La1 76.8(4) . . ? C4 C3 H3A 125.2 . . ? C2 C3 H3A 125.2 . . ? La1 C3 H3A 125.2 . . ? C3 C4 C5 132.0(8) . . ? C3 C4 C9 107.4(6) . . ? C5 C4 C9 120.6(8) . . ? C3 C4 La1 73.5(4) . . ? C5 C4 La1 113.9(5) . . ? C9 C4 La1 77.4(4) . . ? C6 C5 C4 118.4(9) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C5 C6 C7 121.3(9) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C6 122.0(9) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C7 C8 C9 120.0(8) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C1 133.6(6) . . ? C8 C9 C4 117.8(6) . . ? C1 C9 C4 108.6(6) . . ? C8 C9 La1 115.3(4) . . ? C1 C9 La1 75.1(4) . . ? C4 C9 La1 73.6(4) . . ? C1 C10 C18 112.0(6) . . ? C1 C10 C11 111.1(5) . . ? C18 C10 C11 111.4(6) . . ? C1 C10 C17 109.3(6) . . ? C18 C10 C17 107.2(6) . . ? C11 C10 C17 105.6(6) . . ? C12 C11 C10 117.7(6) . . ? C12 C11 H11A 107.9 . . ? C10 C11 H11A 107.9 . . ? C12 C11 H11B 107.9 . . ? C10 C11 H11B 107.9 . . ? H11A C11 H11B 107.2 . . ? N1 C12 C13 120.2(6) . . ? N1 C12 C11 118.3(6) . . ? C13 C12 C11 121.5(6) . . ? C14 C13 C12 120.2(7) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 119.8(7) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 118.8(8) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? N1 C16 C15 122.6(7) . . ? N1 C16 H16 118.7 . . ? C15 C16 H16 118.7 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 C18 H18A 109.5 . . ? C10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C10 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 . . ? Si3' C23' H23D 109.5 . . ? Si3' C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? Si3' C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? Si3' C24' H24D 109.5 . . ? Si3' C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? Si3' C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? Si4 C25 H25A 109.5 . . ? Si4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C31 C27 C30 99(3) 3_756 3_756 ? C31 C27 C32 85(3) 3_756 3_756 ? C30 C27 C32 175(4) 3_756 3_756 ? C31 C27 C32 171(4) 3_756 . ? C30 C27 C32 76(2) 3_756 . ? C32 C27 C32 100(3) 3_756 . ? C31 C27 C28 48.6(19) 3_756 . ? C30 C27 C28 147(2) 3_756 . ? C32 C27 C28 36.7(16) 3_756 . ? C32 C27 C28 136(2) . . ? C31 C27 C33 58(2) 3_756 . ? C30 C27 C33 40.4(17) 3_756 . ? C32 C27 C33 143(3) 3_756 . ? C32 C27 C33 115(2) . . ? C28 C27 C33 107(2) . . ? C31 C27 C27 138(3) 3_756 3_756 ? C30 C27 C27 122(3) 3_756 3_756 ? C32 C27 C27 53.5(17) 3_756 3_756 ? C32 C27 C27 46.2(16) . 3_756 ? C28 C27 C27 90(2) . 3_756 ? C33 C27 C27 159(3) . 3_756 ? C31 C27 C29 142(3) 3_756 3_756 ? C30 C27 C29 43.4(15) 3_756 3_756 ? C32 C27 C29 132(2) 3_756 3_756 ? C32 C27 C29 32.8(12) . 3_756 ? C28 C27 C29 169(2) . 3_756 ? C33 C27 C29 83.4(18) . 3_756 ? C27 C27 C29 78.9(16) 3_756 3_756 ? C32 C28 C31 95(3) 3_756 3_756 ? C32 C28 C29 49(2) 3_756 . ? C31 C28 C29 144(3) 3_756 . ? C32 C28 C27 60(2) 3_756 . ? C31 C28 C27 34.6(18) 3_756 . ? C29 C28 C27 109(2) . . ? C32 C29 C30 78(2) 3_756 . ? C32 C29 C28 37.2(19) 3_756 . ? C30 C29 C28 115(2) . . ? C32 C29 C27 44.4(15) 3_756 3_756 ? C30 C29 C27 33.5(14) . 3_756 ? C28 C29 C27 81.4(16) . 3_756 ? C33 C30 C27 94(3) 3_756 3_756 ? C33 C30 C29 160(4) 3_756 . ? C27 C30 C29 103(3) 3_756 . ? C33 C30 C31 61(2) 3_756 . ? C27 C30 C31 33.4(17) 3_756 . ? C29 C30 C31 136(3) . . ? C33 C30 C32 152(3) 3_756 3_756 ? C27 C30 C32 60.5(16) 3_756 3_756 ? C29 C30 C32 42.7(15) . 3_756 ? C31 C30 C32 94(2) . 3_756 ? C27 C31 C28 97(3) 3_756 3_756 ? C27 C31 C33 90(3) 3_756 3_756 ? C28 C31 C33 171(4) 3_756 3_756 ? C27 C31 C32 60(2) 3_756 . ? C28 C31 C32 36.7(18) 3_756 . ? C33 C31 C32 149(3) 3_756 . ? C27 C31 C30 48(2) 3_756 . ? C28 C31 C30 145(3) 3_756 . ? C33 C31 C30 42.0(15) 3_756 . ? C32 C31 C30 108(2) . . ? C28 C32 C29 94(3) 3_756 3_756 ? C28 C32 C27 83(2) 3_756 3_756 ? C29 C32 C27 177(3) 3_756 3_756 ? C28 C32 C27 162(3) 3_756 . ? C29 C32 C27 103(2) 3_756 . ? C27 C32 C27 80(3) 3_756 . ? C28 C32 C31 48.5(19) 3_756 . ? C29 C32 C31 142(2) 3_756 . ? C27 C32 C31 34.5(16) 3_756 . ? C27 C32 C31 115(2) . . ? C28 C32 C30 153(3) 3_756 3_756 ? C29 C32 C30 59.5(16) 3_756 3_756 ? C27 C32 C30 124(3) 3_756 3_756 ? C27 C32 C30 43.5(13) . 3_756 ? C31 C32 C30 158(2) . 3_756 ? C28 C32 C32 126(3) 3_756 3_756 ? C29 C32 C32 140(3) 3_756 3_756 ? C27 C32 C32 42.8(16) 3_756 3_756 ? C27 C32 C32 37.6(13) . 3_756 ? C31 C32 C32 77.1(18) . 3_756 ? C30 C32 C32 81.0(16) 3_756 3_756 ? C30 C33 C31 76.9(19) 3_756 3_756 ? C30 C33 C27 45.2(17) 3_756 . ? C31 C33 C27 31.9(15) 3_756 . ? 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 La1 Si2 N2 -112.8(3) . . . . ? N1 La1 Si2 N2 117.8(3) . . . . ? C3 La1 Si2 N2 -3.9(4) . . . . ? C2 La1 Si2 N2 25.2(3) . . . . ? C4 La1 Si2 N2 75.4(12) . . . . ? C1 La1 Si2 N2 60.1(3) . . . . ? C9 La1 Si2 N2 90.6(3) . . . . ? Si4 La1 Si2 N2 -140.8(3) . . . . ? Si3' La1 Si2 N2 -86.5(3) . . . . ? Si3 La1 Si2 N2 -85.0(3) . . . . ? N2 La1 Si2 C22 92.8(6) . . . . ? N3 La1 Si2 C22 -19.9(5) . . . . ? N1 La1 Si2 C22 -149.3(5) . . . . ? C3 La1 Si2 C22 89.0(6) . . . . ? C2 La1 Si2 C22 118.0(5) . . . . ? C4 La1 Si2 C22 168.2(12) . . . . ? C1 La1 Si2 C22 153.0(5) . . . . ? C9 La1 Si2 C22 -176.6(5) . . . . ? Si4 La1 Si2 C22 -48.0(5) . . . . ? Si3' La1 Si2 C22 6.3(5) . . . . ? Si3 La1 Si2 C22 7.8(5) . . . . ? N2 La1 Si2 C21 -93.7(5) . . . . ? N3 La1 Si2 C21 153.5(5) . . . . ? N1 La1 Si2 C21 24.1(4) . . . . ? C3 La1 Si2 C21 -97.6(5) . . . . ? C2 La1 Si2 C21 -68.6(5) . . . . ? C4 La1 Si2 C21 -18.4(12) . . . . ? C1 La1 Si2 C21 -33.6(5) . . . . ? C9 La1 Si2 C21 -3.2(5) . . . . ? Si4 La1 Si2 C21 125.5(4) . . . . ? Si3' La1 Si2 C21 179.8(4) . . . . ? Si3 La1 Si2 C21 -178.8(4) . . . . ? N2 La1 Si3 N3 -114.6(4) . . . . ? N1 La1 Si3 N3 -1.0(6) . . . . ? C3 La1 Si3 N3 125.6(4) . . . . ? C2 La1 Si3 N3 144.1(4) . . . . ? C4 La1 Si3 N3 98.5(4) . . . . ? C1 La1 Si3 N3 130.6(4) . . . . ? C9 La1 Si3 N3 98.7(4) . . . . ? Si2 La1 Si3 N3 -84.2(4) . . . . ? Si4 La1 Si3 N3 5.9(4) . . . . ? Si3' La1 Si3 N3 -75.8(9) . . . . ? N2 La1 Si3 C24 150.4(10) . . . . ? N3 La1 Si3 C24 -95.0(10) . . . . ? N1 La1 Si3 C24 -96.0(10) . . . . ? C3 La1 Si3 C24 30.6(10) . . . . ? C2 La1 Si3 C24 49.1(10) . . . . ? C4 La1 Si3 C24 3.5(10) . . . . ? C1 La1 Si3 C24 35.6(10) . . . . ? C9 La1 Si3 C24 3.7(10) . . . . ? Si2 La1 Si3 C24 -179.2(10) . . . . ? Si4 La1 Si3 C24 -89.1(10) . . . . ? Si3' La1 Si3 C24 -170.8(15) . . . . ? N2 La1 Si3 C23 -34.8(9) . . . . ? N3 La1 Si3 C23 79.9(10) . . . . ? N1 La1 Si3 C23 78.8(10) . . . . ? C3 La1 Si3 C23 -154.5(9) . . . . ? C2 La1 Si3 C23 -136.1(9) . . . . ? C4 La1 Si3 C23 178.3(9) . . . . ? C1 La1 Si3 C23 -149.6(9) . . . . ? C9 La1 Si3 C23 178.5(9) . . . . ? Si2 La1 Si3 C23 -4.4(9) . . . . ? Si4 La1 Si3 C23 85.7(9) . . . . ? Si3' La1 Si3 C23 4.0(11) . . . . ? N2 La1 Si3' N3 -133.9(4) . . . . ? N1 La1 Si3' N3 -40.7(5) . . . . ? C3 La1 Si3' N3 105.4(4) . . . . ? C2 La1 Si3' N3 125.9(4) . . . . ? C4 La1 Si3' N3 78.8(4) . . . . ? C1 La1 Si3' N3 114.8(4) . . . . ? C9 La1 Si3' N3 78.5(4) . . . . ? Si2 La1 Si3' N3 -103.7(4) . . . . ? Si4 La1 Si3' N3 -6.7(4) . . . . ? Si3 La1 Si3' N3 84.6(9) . . . . ? N2 La1 Si3' C23' -41.6(10) . . . . ? N3 La1 Si3' C23' 92.4(10) . . . . ? N1 La1 Si3' C23' 51.7(11) . . . . ? C3 La1 Si3' C23' -162.2(10) . . . . ? C2 La1 Si3' C23' -141.7(10) . . . . ? C4 La1 Si3' C23' 171.2(10) . . . . ? C1 La1 Si3' C23' -152.9(10) . . . . ? C9 La1 Si3' C23' 170.8(10) . . . . ? Si2 La1 Si3' C23' -11.3(10) . . . . ? Si4 La1 Si3' C23' 85.7(10) . . . . ? Si3 La1 Si3' C23' 176.9(15) . . . . ? N2 La1 Si3' C24' 146.4(9) . . . . ? N3 La1 Si3' C24' -79.6(10) . . . . ? N1 La1 Si3' C24' -120.3(9) . . . . ? C3 La1 Si3' C24' 25.8(9) . . . . ? C2 La1 Si3' C24' 46.3(9) . . . . ? C4 La1 Si3' C24' -0.8(9) . . . . ? C1 La1 Si3' C24' 35.2(10) . . . . ? C9 La1 Si3' C24' -1.1(9) . . . . ? Si2 La1 Si3' C24' 176.7(9) . . . . ? Si4 La1 Si3' C24' -86.3(9) . . . . ? Si3 La1 Si3' C24' 5.0(11) . . . . ? N2 La1 Si4 N3 71.6(4) . . . . ? N1 La1 Si4 N3 171.5(4) . . . . ? C3 La1 Si4 N3 -66.8(4) . . . . ? C2 La1 Si4 N3 -71.8(4) . . . . ? C4 La1 Si4 N3 -91.8(4) . . . . ? C1 La1 Si4 N3 -111.8(4) . . . . ? C9 La1 Si4 N3 -116.2(4) . . . . ? Si2 La1 Si4 N3 92.9(3) . . . . ? Si3' La1 Si4 N3 6.4(4) . . . . ? Si3 La1 Si4 N3 -5.8(4) . . . . ? N2 La1 Si4 C25 158.8(5) . . . . ? N3 La1 Si4 C25 87.2(6) . . . . ? N1 La1 Si4 C25 -101.3(5) . . . . ? C3 La1 Si4 C25 20.4(5) . . . . ? C2 La1 Si4 C25 15.4(5) . . . . ? C4 La1 Si4 C25 -4.6(5) . . . . ? C1 La1 Si4 C25 -24.6(5) . . . . ? C9 La1 Si4 C25 -29.0(5) . . . . ? Si2 La1 Si4 C25 -179.9(5) . . . . ? Si3' La1 Si4 C25 93.6(5) . . . . ? Si3 La1 Si4 C25 81.4(5) . . . . ? N2 La1 Si4 C26 -20.9(5) . . . . ? N3 La1 Si4 C26 -92.5(6) . . . . ? N1 La1 Si4 C26 79.0(5) . . . . ? C3 La1 Si4 C26 -159.3(5) . . . . ? C2 La1 Si4 C26 -164.2(5) . . . . ? C4 La1 Si4 C26 175.7(5) . . . . ? C1 La1 Si4 C26 155.8(5) . . . . ? C9 La1 Si4 C26 151.3(5) . . . . ? Si2 La1 Si4 C26 0.4(4) . . . . ? Si3' La1 Si4 C26 -86.1(5) . . . . ? Si3 La1 Si4 C26 -98.3(5) . . . . ? N2 La1 N1 C12 -72.3(5) . . . . ? N3 La1 N1 C12 172.8(5) . . . . ? C3 La1 N1 C12 53.6(5) . . . . ? C2 La1 N1 C12 28.4(5) . . . . ? C4 La1 N1 C12 75.7(5) . . . . ? C1 La1 N1 C12 34.0(5) . . . . ? C9 La1 N1 C12 64.3(5) . . . . ? Si2 La1 N1 C12 -98.8(5) . . . . ? Si4 La1 N1 C12 167.6(5) . . . . ? Si3' La1 N1 C12 -164.7(4) . . . . ? Si3 La1 N1 C12 173.4(4) . . . . ? N2 La1 N1 C16 118.6(5) . . . . ? N3 La1 N1 C16 3.6(6) . . . . ? C3 La1 N1 C16 -115.6(5) . . . . ? C2 La1 N1 C16 -140.8(5) . . . . ? C4 La1 N1 C16 -93.4(5) . . . . ? C1 La1 N1 C16 -135.2(5) . . . . ? C9 La1 N1 C16 -104.9(5) . . . . ? Si2 La1 N1 C16 92.0(5) . . . . ? Si4 La1 N1 C16 -1.6(5) . . . . ? Si3' La1 N1 C16 26.2(7) . . . . ? Si3 La1 N1 C16 4.2(8) . . . . ? C22 Si2 N2 Si1 57.0(7) . . . . ? C21 Si2 N2 Si1 -71.9(6) . . . . ? La1 Si2 N2 Si1 176.2(6) . . . . ? C22 Si2 N2 La1 -119.1(5) . . . . ? C21 Si2 N2 La1 111.9(4) . . . . ? C19 Si1 N2 Si2 -51.5(6) . . . . ? C20 Si1 N2 Si2 72.3(6) . . . . ? C19 Si1 N2 La1 124.0(5) . . . . ? C20 Si1 N2 La1 -112.2(4) . . . . ? N3 La1 N2 Si2 73.4(3) . . . . ? N1 La1 N2 Si2 -59.8(3) . . . . ? C3 La1 N2 Si2 177.8(2) . . . . ? C2 La1 N2 Si2 -160.2(3) . . . . ? C4 La1 N2 Si2 -165.7(3) . . . . ? C1 La1 N2 Si2 -131.8(3) . . . . ? C9 La1 N2 Si2 -123.8(3) . . . . ? Si4 La1 N2 Si2 45.8(3) . . . . ? Si3' La1 N2 Si2 93.4(3) . . . . ? Si3 La1 N2 Si2 99.7(3) . . . . ? N3 La1 N2 Si1 -103.1(4) . . . . ? N1 La1 N2 Si1 123.6(3) . . . . ? C3 La1 N2 Si1 1.3(4) . . . . ? C2 La1 N2 Si1 23.3(4) . . . . ? C4 La1 N2 Si1 17.8(6) . . . . ? C1 La1 N2 Si1 51.7(4) . . . . ? C9 La1 N2 Si1 59.6(4) . . . . ? Si2 La1 N2 Si1 -176.5(5) . . . . ? Si4 La1 N2 Si1 -130.7(3) . . . . ? Si3' La1 N2 Si1 -83.2(3) . . . . ? Si3 La1 N2 Si1 -76.9(3) . . . . ? C25 Si4 N3 Si3' 75.3(7) . . . . ? C26 Si4 N3 Si3' -54.0(8) . . . . ? La1 Si4 N3 Si3' -164.7(8) . . . . ? C25 Si4 N3 Si3 45.9(8) . . . . ? C26 Si4 N3 Si3 -83.3(7) . . . . ? La1 Si4 N3 Si3 166.0(8) . . . . ? C25 Si4 N3 La1 -120.0(4) . . . . ? C26 Si4 N3 La1 110.7(5) . . . . ? C23' Si3' N3 Si4 52.4(11) . . . . ? C24' Si3' N3 Si4 -77.5(10) . . . . ? La1 Si3' N3 Si4 164.4(8) . . . . ? C23' Si3' N3 Si3 156.2(14) . . . . ? C24' Si3' N3 Si3 26.2(11) . . . . ? La1 Si3' N3 Si3 -91.9(9) . . . . ? C23' Si3' N3 La1 -111.9(10) . . . . ? C24' Si3' N3 La1 118.1(8) . . . . ? C24 Si3 N3 Si4 -56.2(12) . . . . ? C23 Si3 N3 Si4 73.7(10) . . . . ? La1 Si3 N3 Si4 -165.8(8) . . . . ? C24 Si3 N3 Si3' -153.8(14) . . . . ? C23 Si3 N3 Si3' -24.0(11) . . . . ? La1 Si3 N3 Si3' 96.6(9) . . . . ? C24 Si3 N3 La1 109.6(10) . . . . ? C23 Si3 N3 La1 -120.5(8) . . . . ? N2 La1 N3 Si4 -119.5(3) . . . . ? N1 La1 N3 Si4 -10.9(5) . . . . ? C3 La1 N3 Si4 117.3(3) . . . . ? C2 La1 N3 Si4 127.4(3) . . . . ? C4 La1 N3 Si4 88.6(3) . . . . ? C1 La1 N3 Si4 98.5(4) . . . . ? C9 La1 N3 Si4 74.3(4) . . . . ? Si2 La1 N3 Si4 -90.3(3) . . . . ? Si3' La1 N3 Si4 -168.4(6) . . . . ? Si3 La1 N3 Si4 169.6(6) . . . . ? N2 La1 N3 Si3' 48.9(4) . . . . ? N1 La1 N3 Si3' 157.5(3) . . . . ? C3 La1 N3 Si3' -74.3(4) . . . . ? C2 La1 N3 Si3' -64.3(4) . . . . ? C4 La1 N3 Si3' -103.1(4) . . . . ? C1 La1 N3 Si3' -93.1(4) . . . . ? C9 La1 N3 Si3' -117.3(4) . . . . ? Si2 La1 N3 Si3' 78.1(4) . . . . ? Si4 La1 N3 Si3' 168.4(6) . . . . ? Si3 La1 N3 Si3' -22.0(3) . . . . ? N2 La1 N3 Si3 70.9(4) . . . . ? N1 La1 N3 Si3 179.5(3) . . . . ? C3 La1 N3 Si3 -52.3(4) . . . . ? C2 La1 N3 Si3 -42.3(4) . . . . ? C4 La1 N3 Si3 -81.1(4) . . . . ? C1 La1 N3 Si3 -71.1(5) . . . . ? C9 La1 N3 Si3 -95.3(4) . . . . ? Si2 La1 N3 Si3 100.1(4) . . . . ? Si4 La1 N3 Si3 -169.6(6) . . . . ? Si3' La1 N3 Si3 22.0(3) . . . . ? N2 La1 C1 C2 -81.0(4) . . . . ? N3 La1 C1 C2 61.3(5) . . . . ? N1 La1 C1 C2 -168.3(4) . . . . ? C3 La1 C1 C2 35.7(4) . . . . ? C4 La1 C1 C2 74.8(4) . . . . ? C9 La1 C1 C2 110.9(6) . . . . ? Si2 La1 C1 C2 -108.1(4) . . . . ? Si4 La1 C1 C2 102.1(4) . . . . ? Si3' La1 C1 C2 23.1(5) . . . . ? Si3 La1 C1 C2 29.2(5) . . . . ? N2 La1 C1 C9 168.1(4) . . . . ? N3 La1 C1 C9 -49.7(5) . . . . ? N1 La1 C1 C9 80.7(4) . . . . ? C3 La1 C1 C9 -75.3(4) . . . . ? C2 La1 C1 C9 -110.9(6) . . . . ? C4 La1 C1 C9 -36.2(4) . . . . ? Si2 La1 C1 C9 141.0(3) . . . . ? Si4 La1 C1 C9 -8.9(4) . . . . ? Si3' La1 C1 C9 -87.9(4) . . . . ? Si3 La1 C1 C9 -81.8(4) . . . . ? N2 La1 C1 C10 42.0(5) . . . . ? N3 La1 C1 C10 -175.8(4) . . . . ? N1 La1 C1 C10 -45.4(4) . . . . ? C3 La1 C1 C10 158.6(6) . . . . ? C2 La1 C1 C10 122.9(7) . . . . ? C4 La1 C1 C10 -162.3(6) . . . . ? C9 La1 C1 C10 -126.1(6) . . . . ? Si2 La1 C1 C10 14.9(5) . . . . ? Si4 La1 C1 C10 -135.0(4) . . . . ? Si3' La1 C1 C10 146.0(4) . . . . ? Si3 La1 C1 C10 152.1(4) . . . . ? C9 C1 C2 C3 2.5(7) . . . . ? C10 C1 C2 C3 179.8(6) . . . . ? La1 C1 C2 C3 -67.7(5) . . . . ? C9 C1 C2 La1 70.2(4) . . . . ? C10 C1 C2 La1 -112.5(6) . . . . ? N2 La1 C2 C1 105.6(4) . . . . ? N3 La1 C2 C1 -137.5(4) . . . . ? N1 La1 C2 C1 11.3(4) . . . . ? C3 La1 C2 C1 -116.4(6) . . . . ? C4 La1 C2 C1 -78.5(4) . . . . ? C9 La1 C2 C1 -38.3(4) . . . . ? Si2 La1 C2 C1 93.0(4) . . . . ? Si4 La1 C2 C1 -106.5(4) . . . . ? Si3' La1 C2 C1 -162.6(4) . . . . ? Si3 La1 C2 C1 -155.9(4) . . . . ? N2 La1 C2 C3 -138.0(4) . . . . ? N3 La1 C2 C3 -21.1(5) . . . . ? N1 La1 C2 C3 127.6(4) . . . . ? C4 La1 C2 C3 37.8(4) . . . . ? C1 La1 C2 C3 116.4(6) . . . . ? C9 La1 C2 C3 78.0(5) . . . . ? Si2 La1 C2 C3 -150.6(4) . . . . ? Si4 La1 C2 C3 9.8(5) . . . . ? Si3' La1 C2 C3 -46.3(4) . . . . ? Si3 La1 C2 C3 -39.6(4) . . . . ? C1 C2 C3 C4 -2.3(8) . . . . ? La1 C2 C3 C4 -72.4(5) . . . . ? C1 C2 C3 La1 70.1(5) . . . . ? N2 La1 C3 C4 161.2(4) . . . . ? N3 La1 C3 C4 -86.8(4) . . . . ? N1 La1 C3 C4 51.0(5) . . . . ? C2 La1 C3 C4 111.3(6) . . . . ? C1 La1 C3 C4 76.5(4) . . . . ? C9 La1 C3 C4 37.4(4) . . . . ? Si2 La1 C3 C4 163.4(3) . . . . ? Si4 La1 C3 C4 -61.3(4) . . . . ? Si3' La1 C3 C4 -112.7(4) . . . . ? Si3 La1 C3 C4 -109.0(4) . . . . ? N2 La1 C3 C2 49.8(5) . . . . ? N3 La1 C3 C2 161.9(4) . . . . ? N1 La1 C3 C2 -60.3(5) . . . . ? C4 La1 C3 C2 -111.3(6) . . . . ? C1 La1 C3 C2 -34.8(4) . . . . ? C9 La1 C3 C2 -74.0(4) . . . . ? Si2 La1 C3 C2 52.1(6) . . . . ? Si4 La1 C3 C2 -172.7(4) . . . . ? Si3' La1 C3 C2 136.0(4) . . . . ? Si3 La1 C3 C2 139.6(4) . . . . ? C2 C3 C4 C5 179.3(7) . . . . ? La1 C3 C4 C5 107.5(8) . . . . ? C2 C3 C4 C9 1.1(7) . . . . ? La1 C3 C4 C9 -70.7(5) . . . . ? C2 C3 C4 La1 71.8(5) . . . . ? N2 La1 C4 C3 -30.6(6) . . . . ? N3 La1 C4 C3 94.3(4) . . . . ? N1 La1 C4 C3 -135.3(4) . . . . ? C2 La1 C4 C3 -38.0(4) . . . . ? C1 La1 C4 C3 -76.8(4) . . . . ? C9 La1 C4 C3 -112.6(6) . . . . ? Si2 La1 C4 C3 -93.8(12) . . . . ? Si4 La1 C4 C3 122.2(4) . . . . ? Si3' La1 C4 C3 68.0(4) . . . . ? Si3 La1 C4 C3 67.0(4) . . . . ? N2 La1 C4 C5 -159.9(6) . . . . ? N3 La1 C4 C5 -35.0(7) . . . . ? N1 La1 C4 C5 95.4(7) . . . . ? C3 La1 C4 C5 -129.3(9) . . . . ? C2 La1 C4 C5 -167.3(8) . . . . ? C1 La1 C4 C5 154.0(8) . . . . ? C9 La1 C4 C5 118.1(8) . . . . ? Si2 La1 C4 C5 137.0(10) . . . . ? Si4 La1 C4 C5 -7.1(7) . . . . ? Si3' La1 C4 C5 -61.3(7) . . . . ? Si3 La1 C4 C5 -62.3(7) . . . . ? N2 La1 C4 C9 82.0(5) . . . . ? N3 La1 C4 C9 -153.1(4) . . . . ? N1 La1 C4 C9 -22.7(4) . . . . ? C3 La1 C4 C9 112.6(6) . . . . ? C2 La1 C4 C9 74.6(4) . . . . ? C1 La1 C4 C9 35.9(4) . . . . ? Si2 La1 C4 C9 18.9(14) . . . . ? Si4 La1 C4 C9 -125.2(4) . . . . ? Si3' La1 C4 C9 -179.4(4) . . . . ? Si3 La1 C4 C9 179.6(4) . . . . ? C3 C4 C5 C6 -178.2(8) . . . . ? C9 C4 C5 C6 -0.2(11) . . . . ? La1 C4 C5 C6 -89.3(8) . . . . ? C4 C5 C6 C7 -0.1(13) . . . . ? C5 C6 C7 C8 0.6(14) . . . . ? C6 C7 C8 C9 -0.8(12) . . . . ? C7 C8 C9 C1 177.9(7) . . . . ? C7 C8 C9 C4 0.5(10) . . . . ? C7 C8 C9 La1 84.6(7) . . . . ? C2 C1 C9 C8 -179.4(7) . . . . ? C10 C1 C9 C8 3.5(12) . . . . ? La1 C1 C9 C8 -111.0(7) . . . . ? C2 C1 C9 C4 -1.8(7) . . . . ? C10 C1 C9 C4 -179.0(6) . . . . ? La1 C1 C9 C4 66.6(4) . . . . ? C2 C1 C9 La1 -68.4(4) . . . . ? C10 C1 C9 La1 114.4(6) . . . . ? C3 C4 C9 C8 178.5(6) . . . . ? C5 C4 C9 C8 0.0(10) . . . . ? La1 C4 C9 C8 110.5(6) . . . . ? C3 C4 C9 C1 0.5(7) . . . . ? C5 C4 C9 C1 -178.0(6) . . . . ? La1 C4 C9 C1 -67.5(4) . . . . ? C3 C4 C9 La1 68.0(5) . . . . ? C5 C4 C9 La1 -110.5(6) . . . . ? N2 La1 C9 C8 115.5(5) . . . . ? N3 La1 C9 C8 -83.0(5) . . . . ? N1 La1 C9 C8 42.4(5) . . . . ? C3 La1 C9 C8 -150.7(6) . . . . ? C2 La1 C9 C8 169.3(6) . . . . ? C4 La1 C9 C8 -113.5(7) . . . . ? C1 La1 C9 C8 131.5(7) . . . . ? Si2 La1 C9 C8 70.9(6) . . . . ? Si4 La1 C9 C8 -55.0(5) . . . . ? Si3' La1 C9 C8 -112.8(5) . . . . ? Si3 La1 C9 C8 -113.9(5) . . . . ? N2 La1 C9 C1 -16.0(5) . . . . ? N3 La1 C9 C1 145.5(4) . . . . ? N1 La1 C9 C1 -89.1(4) . . . . ? C3 La1 C9 C1 77.8(4) . . . . ? C2 La1 C9 C1 37.8(4) . . . . ? C4 La1 C9 C1 115.0(6) . . . . ? Si2 La1 C9 C1 -60.7(4) . . . . ? Si4 La1 C9 C1 173.5(3) . . . . ? Si3' La1 C9 C1 115.7(4) . . . . ? Si3 La1 C9 C1 114.5(4) . . . . ? N2 La1 C9 C4 -131.0(4) . . . . ? N3 La1 C9 C4 30.5(5) . . . . ? N1 La1 C9 C4 155.9(4) . . . . ? C3 La1 C9 C4 -37.2(4) . . . . ? C2 La1 C9 C4 -77.2(4) . . . . ? C1 La1 C9 C4 -115.0(6) . . . . ? Si2 La1 C9 C4 -175.6(3) . . . . ? Si4 La1 C9 C4 58.5(4) . . . . ? Si3' La1 C9 C4 0.7(5) . . . . ? Si3 La1 C9 C4 -0.5(4) . . . . ? C2 C1 C10 C18 -133.2(7) . . . . ? C9 C1 C10 C18 43.5(9) . . . . ? La1 C1 C10 C18 137.4(5) . . . . ? C2 C1 C10 C11 101.5(7) . . . . ? C9 C1 C10 C11 -81.9(8) . . . . ? La1 C1 C10 C11 12.1(7) . . . . ? C2 C1 C10 C17 -14.5(9) . . . . ? C9 C1 C10 C17 162.1(6) . . . . ? La1 C1 C10 C17 -104.0(5) . . . . ? C1 C10 C11 C12 63.6(8) . . . . ? C18 C10 C11 C12 -62.1(8) . . . . ? C17 C10 C11 C12 -178.1(6) . . . . ? C16 N1 C12 C13 -1.4(10) . . . . ? La1 N1 C12 C13 -170.5(5) . . . . ? C16 N1 C12 C11 -179.6(6) . . . . ? La1 N1 C12 C11 11.3(8) . . . . ? C10 C11 C12 N1 -85.2(8) . . . . ? C10 C11 C12 C13 96.6(8) . . . . ? N1 C12 C13 C14 1.0(11) . . . . ? C11 C12 C13 C14 179.2(7) . . . . ? C12 C13 C14 C15 -0.2(13) . . . . ? C13 C14 C15 C16 -0.3(13) . . . . ? C12 N1 C16 C15 1.0(11) . . . . ? La1 N1 C16 C15 170.6(6) . . . . ? C14 C15 C16 N1 -0.1(13) . . . . ? C31 C27 C28 C32 -178(7) 3_756 . . 3_756 ? C30 C27 C28 C32 -174(8) 3_756 . . 3_756 ? C32 C27 C28 C32 -8(6) . . . 3_756 ? C33 C27 C28 C32 -172(4) . . . 3_756 ? C27 C27 C28 C32 -5(4) 3_756 . . 3_756 ? C29 C27 C28 C32 -20(14) 3_756 . . 3_756 ? C30 C27 C28 C31 4(6) 3_756 . . 3_756 ? C32 C27 C28 C31 178(7) 3_756 . . 3_756 ? C32 C27 C28 C31 169(7) . . . 3_756 ? C33 C27 C28 C31 6(4) . . . 3_756 ? C27 C27 C28 C31 173(6) 3_756 . . 3_756 ? C29 C27 C28 C31 158(15) 3_756 . . 3_756 ? C31 C27 C28 C29 -177(5) 3_756 . . . ? C30 C27 C28 C29 -173(6) 3_756 . . . ? C32 C27 C28 C29 0(3) 3_756 . . . ? C32 C27 C28 C29 -8(5) . . . . ? C33 C27 C28 C29 -172(2) . . . . ? C27 C27 C28 C29 -4(3) 3_756 . . . ? C29 C27 C28 C29 -19(15) 3_756 . . . ? C31 C28 C29 C32 -3(6) 3_756 . . 3_756 ? C27 C28 C29 C32 -1(4) . . . 3_756 ? C32 C28 C29 C30 3(5) 3_756 . . . ? C31 C28 C29 C30 0(8) 3_756 . . . ? C27 C28 C29 C30 3(4) . . . . ? C32 C28 C29 C27 4(4) 3_756 . . 3_756 ? C31 C28 C29 C27 1(6) 3_756 . . 3_756 ? C27 C28 C29 C27 4(3) . . . 3_756 ? C32 C29 C30 C33 -147(12) 3_756 . . 3_756 ? C28 C29 C30 C33 -149(11) . . . 3_756 ? C27 C29 C30 C33 -151(14) 3_756 . . 3_756 ? C32 C29 C30 C27 4(4) 3_756 . . 3_756 ? C28 C29 C30 C27 2(4) . . . 3_756 ? C32 C29 C30 C31 1(5) 3_756 . . . ? C28 C29 C30 C31 -1(5) . . . . ? C27 C29 C30 C31 -3(3) 3_756 . . . ? C28 C29 C30 C32 -2(3) . . . 3_756 ? C27 C29 C30 C32 -4(4) 3_756 . . 3_756 ? C33 C30 C31 C27 174(6) 3_756 . . 3_756 ? C29 C30 C31 C27 6(6) . . . 3_756 ? C32 C30 C31 C27 6(4) 3_756 . . 3_756 ? C33 C30 C31 C28 170(7) 3_756 . . 3_756 ? C27 C30 C31 C28 -4(6) 3_756 . . 3_756 ? C29 C30 C31 C28 2(9) . . . 3_756 ? C32 C30 C31 C28 3(7) 3_756 . . 3_756 ? C27 C30 C31 C33 -174(6) 3_756 . . 3_756 ? C29 C30 C31 C33 -168(6) . . . 3_756 ? C32 C30 C31 C33 -167(4) 3_756 . . 3_756 ? C33 C30 C31 C32 171(4) 3_756 . . . ? C27 C30 C31 C32 -3(4) 3_756 . . . ? C29 C30 C31 C32 3(5) . . . . ? C32 C30 C31 C32 3(3) 3_756 . . . ? C31 C27 C32 C28 142(25) 3_756 . . 3_756 ? C30 C27 C32 C28 -163(15) 3_756 . . 3_756 ? C32 C27 C32 C28 20(15) 3_756 . . 3_756 ? C28 C27 C32 C28 25(18) . . . 3_756 ? C33 C27 C32 C28 -173(14) . . . 3_756 ? C27 C27 C32 C28 20(15) 3_756 . . 3_756 ? C29 C27 C32 C28 -159(17) 3_756 . . 3_756 ? C31 C27 C32 C29 -58(27) 3_756 . . 3_756 ? C30 C27 C32 C29 -4(4) 3_756 . . 3_756 ? C32 C27 C32 C29 179(4) 3_756 . . 3_756 ? C28 C27 C32 C29 -176(4) . . . 3_756 ? C33 C27 C32 C29 -13(4) . . . 3_756 ? C27 C27 C32 C29 179(4) 3_756 . . 3_756 ? C31 C27 C32 C27 123(27) 3_756 . . 3_756 ? C30 C27 C32 C27 177(4) 3_756 . . 3_756 ? C32 C27 C32 C27 0.000(3) 3_756 . . 3_756 ? C28 C27 C32 C27 5(4) . . . 3_756 ? C33 C27 C32 C27 168(4) . . . 3_756 ? C29 C27 C32 C27 -179(4) 3_756 . . 3_756 ? C31 C27 C32 C31 127(24) 3_756 . . . ? C30 C27 C32 C31 -178(3) 3_756 . . . ? C32 C27 C32 C31 5(3) 3_756 . . . ? C28 C27 C32 C31 10(6) . . . . ? C33 C27 C32 C31 172(2) . . . . ? C27 C27 C32 C31 5(3) 3_756 . . . ? C29 C27 C32 C31 -174(5) 3_756 . . . ? C31 C27 C32 C30 -54(25) 3_756 . . 3_756 ? C32 C27 C32 C30 -177(4) 3_756 . . 3_756 ? C28 C27 C32 C30 -172(6) . . . 3_756 ? C33 C27 C32 C30 -9(2) . . . 3_756 ? C27 C27 C32 C30 -177(4) 3_756 . . 3_756 ? C29 C27 C32 C30 4(4) 3_756 . . 3_756 ? C31 C27 C32 C32 123(27) 3_756 . . 3_756 ? C30 C27 C32 C32 177(4) 3_756 . . 3_756 ? C28 C27 C32 C32 5(4) . . . 3_756 ? C33 C27 C32 C32 168(4) . . . 3_756 ? C27 C27 C32 C32 0.000(3) 3_756 . . 3_756 ? C29 C27 C32 C32 -179(4) 3_756 . . 3_756 ? C27 C31 C32 C28 178(7) 3_756 . . 3_756 ? C33 C31 C32 C28 -167(8) 3_756 . . 3_756 ? C30 C31 C32 C28 -179(5) . . . 3_756 ? C27 C31 C32 C29 -179(7) 3_756 . . 3_756 ? C28 C31 C32 C29 3(5) 3_756 . . 3_756 ? C33 C31 C32 C29 -164(6) 3_756 . . 3_756 ? C30 C31 C32 C29 -176(5) . . . 3_756 ? C28 C31 C32 C27 -178(7) 3_756 . . 3_756 ? C33 C31 C32 C27 15(5) 3_756 . . 3_756 ? C30 C31 C32 C27 3(3) . . . 3_756 ? C27 C31 C32 C27 -8(6) 3_756 . . . ? C28 C31 C32 C27 174(6) 3_756 . . . ? C33 C31 C32 C27 7(8) 3_756 . . . ? C30 C31 C32 C27 -5(4) . . . . ? C27 C31 C32 C30 -11(9) 3_756 . . 3_756 ? C28 C31 C32 C30 171(10) 3_756 . . 3_756 ? C33 C31 C32 C30 4(12) 3_756 . . 3_756 ? C30 C31 C32 C30 -8(9) . . . 3_756 ? C27 C31 C32 C32 -5(4) 3_756 . . 3_756 ? C28 C31 C32 C32 177(5) 3_756 . . 3_756 ? C33 C31 C32 C32 10(6) 3_756 . . 3_756 ? C30 C31 C32 C32 -2(3) . . . 3_756 ? C31 C27 C33 C30 -174(7) 3_756 . . 3_756 ? C32 C27 C33 C30 173(7) 3_756 . . 3_756 ? C32 C27 C33 C30 14(4) . . . 3_756 ? C28 C27 C33 C30 -179(5) . . . 3_756 ? C27 C27 C33 C30 39(9) 3_756 . . 3_756 ? C29 C27 C33 C30 7(3) 3_756 . . 3_756 ? C30 C27 C33 C31 174(7) 3_756 . . 3_756 ? C32 C27 C33 C31 -13(4) 3_756 . . 3_756 ? C32 C27 C33 C31 -173(6) . . . 3_756 ? C28 C27 C33 C31 -5(4) . . . 3_756 ? C27 C27 C33 C31 -147(12) 3_756 . . 3_756 ? C29 C27 C33 C31 -180(5) 3_756 . . 3_756 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.058 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.074 data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 900281' #TrackingRef 'CCDC 900280.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H46 N3 Si4 Sm' _chemical_formula_sum 'C26 H46 N3 Si4 Sm' _chemical_formula_weight 663.37 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.4325(19) _cell_length_b 8.3392(9) _cell_length_c 22.810(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.839(3) _cell_angle_gamma 90.00 _cell_volume 3311.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14089 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 1.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.417 _exptl_absorpt_correction_T_max 0.695 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21131 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7527 _reflns_number_gt 5988 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+13.5187P] 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 7527 _refine_ls_number_parameters 288 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1706 _refine_ls_wR_factor_gt 0.1493 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.095 _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 Sm1 Sm 0.73545(2) 0.26433(4) 0.847849(15) 0.04687(14) Uani 1 1 d . A . Si1 Si 0.91942(12) 0.3209(3) 0.93094(9) 0.0571(5) Uani 1 1 d D . . H1 H 0.899(4) 0.486(3) 0.913(3) 0.07(2) Uiso 1 1 d D . . Si2 Si 0.83621(15) 0.0066(3) 0.91343(11) 0.0704(7) Uani 1 1 d D . . H2 H 0.7617(19) -0.028(8) 0.882(3) 0.06(2) Uiso 1 1 d D . . Si3 Si 0.6366(3) 0.4142(7) 0.9744(2) 0.0763(10) Uiso 0.50 1 d PD A 1 H3 H 0.588(8) 0.559(11) 0.974(7) 0.092 Uiso 0.50 1 d PD B 1 Si3' Si 0.6677(3) 0.3596(7) 0.9860(2) 0.0763(10) Uiso 0.50 1 d PD A 2 H3' H 0.698(10) 0.267(17) 1.037(5) 0.092 Uiso 0.50 1 d PD C 2 Si4 Si 0.58217(14) 0.1367(3) 0.89690(11) 0.0676(6) Uani 1 1 d D . . H4 H 0.605(3) 0.101(7) 0.8366(10) 0.043(17) Uiso 1 1 d D . . N1 N 0.7616(3) 0.0704(7) 0.7622(3) 0.0550(14) Uani 1 1 d . . . N2 N 0.8469(3) 0.2057(7) 0.9018(3) 0.0524(14) Uani 1 1 d . A . N3 N 0.6498(4) 0.2686(7) 0.9212(3) 0.0607(16) Uani 1 1 d D A . C1 C 0.7815(5) 0.4568(11) 0.7574(4) 0.0760(8) Uani 1 1 d . . . C2 C 0.7858(5) 0.5528(11) 0.8086(4) 0.0760(8) Uani 1 1 d . A . H2A H 0.8333 0.6066 0.8241 0.091 Uiso 1 1 calc R . . C3 C 0.7140(5) 0.5814(11) 0.8289(4) 0.0760(8) Uani 1 1 d . . . H3A H 0.7025 0.6607 0.8595 0.091 Uiso 1 1 calc R D . C4 C 0.6595(5) 0.5111(11) 0.7902(4) 0.0760(8) Uani 1 1 d . A . C5 C 0.5777(5) 0.5010(11) 0.7884(4) 0.0760(8) Uani 1 1 d . . . H5 H 0.5497 0.5530 0.8170 0.091 Uiso 1 1 calc R D . C6 C 0.5418(6) 0.4176(11) 0.7461(4) 0.0760(8) Uani 1 1 d . D . H6 H 0.4880 0.4119 0.7456 0.091 Uiso 1 1 calc R . . C7 C 0.5799(5) 0.3365(11) 0.7015(4) 0.0760(8) Uani 1 1 d . . . H7 H 0.5512 0.2785 0.6727 0.091 Uiso 1 1 calc R D . C8 C 0.6590(5) 0.3416(12) 0.6999(4) 0.0760(8) Uani 1 1 d . A . H8 H 0.6847 0.2867 0.6707 0.091 Uiso 1 1 calc R . . C9 C 0.7006(5) 0.4329(11) 0.7441(4) 0.0760(8) Uani 1 1 d . A . C10 C 0.8497(5) 0.4027(11) 0.7233(3) 0.067(2) Uani 1 1 d . D . C11 C 0.8746(5) 0.2304(11) 0.7395(4) 0.069(2) Uani 1 1 d . . . H11A H 0.9220 0.2066 0.7198 0.083 Uiso 1 1 calc R D . H11B H 0.8867 0.2261 0.7819 0.083 Uiso 1 1 calc R . . C12 C 0.8172(5) 0.1010(10) 0.7239(3) 0.065(2) Uani 1 1 d . D . C13 C 0.8225(7) 0.0109(13) 0.6737(4) 0.090(3) Uani 1 1 d . . . H13 H 0.8613 0.0327 0.6476 0.108 Uiso 1 1 calc R D . C14 C 0.7713(8) -0.1105(13) 0.6617(4) 0.102(4) Uani 1 1 d . D . H14 H 0.7741 -0.1711 0.6272 0.122 Uiso 1 1 calc R . . C15 C 0.7158(7) -0.1431(11) 0.7005(4) 0.083(3) Uani 1 1 d . . . H15 H 0.6805 -0.2268 0.6931 0.100 Uiso 1 1 calc R D . C16 C 0.7125(5) -0.0511(9) 0.7507(4) 0.066(2) Uani 1 1 d . D . H16 H 0.6749 -0.0742 0.7776 0.080 Uiso 1 1 calc R . . C17 C 0.9204(5) 0.5107(14) 0.7411(4) 0.097(3) Uani 1 1 d . . . H17A H 0.9094 0.6207 0.7297 0.145 Uiso 1 1 calc R D . H17B H 0.9650 0.4731 0.7213 0.145 Uiso 1 1 calc R . . H17C H 0.9307 0.5051 0.7832 0.145 Uiso 1 1 calc R . . C18 C 0.8339(5) 0.4202(12) 0.6570(4) 0.079(3) Uani 1 1 d . . . H18A H 0.7933 0.3468 0.6441 0.118 Uiso 1 1 calc R D . H18B H 0.8802 0.3955 0.6369 0.118 Uiso 1 1 calc R . . H18C H 0.8181 0.5294 0.6480 0.118 Uiso 1 1 calc R . . C19 C 0.9337(7) 0.2993(15) 1.0121(4) 0.107(4) Uani 1 1 d . . . H19A H 0.8871 0.3306 1.0306 0.160 Uiso 1 1 calc R . . H19B H 0.9757 0.3675 1.0262 0.160 Uiso 1 1 calc R . . H19C H 0.9457 0.1885 1.0217 0.160 Uiso 1 1 calc R . . C20 C 1.0132(6) 0.2816(14) 0.8986(6) 0.106(4) Uani 1 1 d . . . H20A H 1.0285 0.1715 0.9065 0.159 Uiso 1 1 calc R . . H20B H 1.0516 0.3538 0.9159 0.159 Uiso 1 1 calc R . . H20C H 1.0084 0.2989 0.8565 0.159 Uiso 1 1 calc R . . C21 C 0.9082(6) -0.1205(12) 0.8774(6) 0.116(4) Uani 1 1 d . D . H21A H 0.9005 -0.1119 0.8352 0.173 Uiso 1 1 calc R . . H21B H 0.9019 -0.2314 0.8892 0.173 Uiso 1 1 calc R . . H21C H 0.9595 -0.0844 0.8893 0.173 Uiso 1 1 calc R . . C22 C 0.8099(16) -0.059(7) 0.9886(9) 0.123(9) Uani 0.50 1 d PD D 1 H22A H 0.8510 -0.0308 1.0170 0.184 Uiso 0.50 1 calc PR D 1 H22B H 0.8023 -0.1742 0.9889 0.184 Uiso 0.50 1 calc PR D 1 H22C H 0.7629 -0.0058 0.9988 0.184 Uiso 0.50 1 calc PR D 1 C22' C 0.8408(17) -0.059(7) 0.9919(10) 0.123(9) Uani 0.50 1 d PD D 2 H22D H 0.8922 -0.0419 1.0089 0.184 Uiso 0.50 1 calc PR D 2 H22E H 0.8281 -0.1723 0.9940 0.184 Uiso 0.50 1 calc PR D 2 H22F H 0.8043 0.0023 1.0135 0.184 Uiso 0.50 1 calc PR D 2 C23 C 0.6257(18) 0.289(3) 1.0435(10) 0.122(7) Uiso 0.50 1 d PD A 1 H23A H 0.5761 0.2363 1.0415 0.182 Uiso 0.50 1 calc PR A 1 H23B H 0.6296 0.3581 1.0777 0.182 Uiso 0.50 1 calc PR A 1 H23C H 0.6661 0.2088 1.0465 0.182 Uiso 0.50 1 calc PR A 1 C23' C 0.5929(14) 0.345(4) 1.0414(11) 0.122(7) Uiso 0.50 1 d PD A 2 H23D H 0.5426 0.3613 1.0222 0.182 Uiso 0.50 1 calc PR A 2 H23E H 0.6021 0.4273 1.0711 0.182 Uiso 0.50 1 calc PR A 2 H23F H 0.5952 0.2404 1.0597 0.182 Uiso 0.50 1 calc PR A 2 C24 C 0.7374(11) 0.480(3) 0.9981(13) 0.120(6) Uiso 0.50 1 d PD A 1 H24A H 0.7686 0.3866 1.0077 0.179 Uiso 0.50 1 calc PR A 1 H24B H 0.7355 0.5489 1.0323 0.179 Uiso 0.50 1 calc PR A 1 H24C H 0.7596 0.5387 0.9664 0.179 Uiso 0.50 1 calc PR A 1 C24' C 0.7188(15) 0.549(2) 0.9889(13) 0.120(6) Uiso 0.50 1 d PD A 2 H24D H 0.7662 0.5390 0.9687 0.179 Uiso 0.50 1 calc PR A 2 H24E H 0.7305 0.5786 1.0296 0.179 Uiso 0.50 1 calc PR A 2 H24F H 0.6871 0.6319 0.9701 0.179 Uiso 0.50 1 calc PR A 2 C25 C 0.4816(5) 0.2102(14) 0.8890(5) 0.091(3) Uani 1 1 d . D . H25A H 0.4617 0.2258 0.9275 0.137 Uiso 1 1 calc R . . H25B H 0.4502 0.1319 0.8674 0.137 Uiso 1 1 calc R . . H25C H 0.4803 0.3112 0.8679 0.137 Uiso 1 1 calc R . . C26 C 0.5833(6) -0.0600(12) 0.9345(5) 0.102(3) Uani 1 1 d . D . H26A H 0.6356 -0.1001 0.9381 0.153 Uiso 1 1 calc R . . H26B H 0.5515 -0.1352 0.9119 0.153 Uiso 1 1 calc R . . H26C H 0.5636 -0.0478 0.9733 0.153 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0539(2) 0.0475(2) 0.0392(2) 0.00555(14) 0.00115(15) -0.00508(15) Si1 0.0591(12) 0.0550(12) 0.0562(12) -0.0031(10) -0.0074(9) -0.0095(10) Si2 0.0853(16) 0.0513(12) 0.0708(15) 0.0141(11) -0.0329(12) -0.0157(11) Si4 0.0630(13) 0.0744(15) 0.0666(14) -0.0019(12) 0.0137(11) -0.0102(12) N1 0.062(4) 0.056(4) 0.046(3) -0.001(3) -0.002(3) 0.003(3) N2 0.059(3) 0.044(3) 0.052(3) 0.000(3) -0.010(3) -0.005(3) N3 0.067(4) 0.061(4) 0.055(4) 0.003(3) 0.011(3) -0.011(3) C1 0.0825(19) 0.076(2) 0.0701(19) 0.0230(15) 0.0094(15) 0.0062(17) C2 0.0825(19) 0.076(2) 0.0701(19) 0.0230(15) 0.0094(15) 0.0062(17) C3 0.0825(19) 0.076(2) 0.0701(19) 0.0230(15) 0.0094(15) 0.0062(17) C4 0.0825(19) 0.076(2) 0.0701(19) 0.0230(15) 0.0094(15) 0.0062(17) C5 0.0825(19) 0.076(2) 0.0701(19) 0.0230(15) 0.0094(15) 0.0062(17) C6 0.0825(19) 0.076(2) 0.0701(19) 0.0230(15) 0.0094(15) 0.0062(17) C7 0.0825(19) 0.076(2) 0.0701(19) 0.0230(15) 0.0094(15) 0.0062(17) C8 0.0825(19) 0.076(2) 0.0701(19) 0.0230(15) 0.0094(15) 0.0062(17) C9 0.0825(19) 0.076(2) 0.0701(19) 0.0230(15) 0.0094(15) 0.0062(17) C10 0.070(5) 0.081(6) 0.051(4) 0.018(4) 0.016(4) -0.011(4) C11 0.047(4) 0.100(7) 0.061(5) 0.016(4) 0.006(4) 0.000(4) C12 0.077(5) 0.069(5) 0.049(4) 0.009(4) 0.008(4) 0.024(4) C13 0.124(9) 0.080(7) 0.068(6) -0.001(5) 0.028(6) 0.023(6) C14 0.179(12) 0.070(7) 0.056(6) -0.001(5) 0.009(7) 0.023(7) C15 0.136(9) 0.050(5) 0.060(5) 0.000(4) -0.021(5) 0.007(5) C16 0.082(6) 0.052(4) 0.063(5) 0.007(4) -0.010(4) 0.005(4) C17 0.078(6) 0.124(9) 0.089(7) 0.018(6) 0.016(5) -0.034(6) C18 0.087(6) 0.095(7) 0.056(5) 0.019(5) 0.018(4) -0.002(5) C19 0.129(9) 0.120(9) 0.069(6) -0.003(6) -0.021(6) -0.054(8) C20 0.067(6) 0.131(10) 0.120(10) -0.031(7) 0.014(6) -0.020(6) C21 0.091(7) 0.059(6) 0.192(13) -0.012(7) -0.043(8) 0.008(5) C22 0.14(2) 0.123(10) 0.099(9) 0.066(8) -0.100(12) -0.09(2) C22' 0.14(2) 0.123(10) 0.099(9) 0.066(8) -0.100(12) -0.09(2) C25 0.067(6) 0.120(9) 0.088(7) -0.010(6) 0.017(5) -0.005(6) C26 0.103(8) 0.084(7) 0.121(9) 0.013(7) 0.020(7) -0.026(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 Sm1 N3 2.297(6) . ? Sm1 N2 2.300(6) . ? Sm1 N1 2.593(6) . ? Sm1 C3 2.702(9) . ? Sm1 C2 2.727(9) . ? Sm1 C4 2.747(9) . ? Sm1 C1 2.765(8) . ? Sm1 C9 2.794(8) . ? Sm1 Si2 3.112(2) . ? Sm1 Si4 3.134(2) . ? Sm1 H2 2.60(7) . ? Si1 N2 1.697(6) . ? Si1 C20 1.855(10) . ? Si1 C19 1.865(10) . ? Si1 H1 1.479(10) . ? Si2 N2 1.694(6) . ? Si2 C21 1.863(11) . ? Si2 C22' 1.871(16) . ? Si2 C22 1.878(17) . ? Si2 H2 1.479(10) . ? Si3 N3 1.740(8) . ? Si3 C24 1.894(16) . ? Si3 C23 1.909(17) . ? Si3 H3 1.478(10) . ? Si3' N3 1.676(8) . ? Si3' C24' 1.816(16) . ? Si3' C23' 1.862(16) . ? Si3' H3' 1.480(10) . ? Si4 N3 1.686(7) . ? Si4 C26 1.851(10) . ? Si4 C25 1.858(10) . ? Si4 H4 1.480(10) . ? N1 C16 1.344(10) . ? N1 C12 1.360(10) . ? C1 C2 1.415(13) . ? C1 C9 1.441(12) . ? C1 C10 1.520(12) . ? C2 C3 1.377(12) . ? C2 H2A 0.9900 . ? C3 C4 1.393(13) . ? C3 H3A 0.9900 . ? C4 C5 1.427(12) . ? C4 C9 1.455(13) . ? C5 C6 1.321(12) . ? C5 H5 0.9400 . ? C6 C7 1.414(12) . ? C6 H6 0.9400 . ? C7 C8 1.382(12) . ? C7 H7 0.9400 . ? C8 C9 1.431(13) . ? C8 H8 0.9400 . ? C10 C18 1.532(11) . ? C10 C11 1.540(12) . ? C10 C17 1.563(12) . ? C11 C12 1.502(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.377(12) . ? C13 C14 1.369(15) . ? C13 H13 0.9400 . ? C14 C15 1.369(14) . ? C14 H14 0.9400 . ? C15 C16 1.382(11) . ? C15 H15 0.9400 . ? C16 H16 0.9400 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C22' H22D 0.9700 . ? C22' H22E 0.9700 . ? C22' H22F 0.9700 . ? C23 H3' 1.28(18) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C23' H23D 0.9700 . ? C23' H23E 0.9700 . ? C23' H23F 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C24' H24D 0.9700 . ? C24' H24E 0.9700 . ? C24' H24F 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Sm1 N2 100.1(2) . . ? N3 Sm1 N1 134.7(2) . . ? N2 Sm1 N1 95.4(2) . . ? N3 Sm1 C3 90.7(2) . . ? N2 Sm1 C3 113.6(3) . . ? N1 Sm1 C3 121.2(2) . . ? N3 Sm1 C2 117.2(2) . . ? N2 Sm1 C2 94.9(2) . . ? N1 Sm1 C2 103.4(2) . . ? C3 Sm1 C2 29.4(2) . . ? N3 Sm1 C4 91.3(2) . . ? N2 Sm1 C4 142.2(3) . . ? N1 Sm1 C4 101.8(2) . . ? C3 Sm1 C4 29.6(3) . . ? C2 Sm1 C4 48.5(3) . . ? N3 Sm1 C1 139.3(3) . . ? N2 Sm1 C1 104.7(2) . . ? N1 Sm1 C1 74.4(3) . . ? C3 Sm1 C1 49.9(3) . . ? C2 Sm1 C1 29.9(3) . . ? C4 Sm1 C1 50.1(3) . . ? N3 Sm1 C9 119.2(3) . . ? N2 Sm1 C9 134.6(2) . . ? N1 Sm1 C9 73.4(2) . . ? C3 Sm1 C9 49.4(3) . . ? C2 Sm1 C9 48.5(3) . . ? C4 Sm1 C9 30.4(3) . . ? C1 Sm1 C9 30.1(3) . . ? N3 Sm1 Si2 91.84(18) . . ? N2 Sm1 Si2 32.26(15) . . ? N1 Sm1 Si2 79.35(14) . . ? C3 Sm1 Si2 145.4(2) . . ? C2 Sm1 Si2 125.7(2) . . ? C4 Sm1 Si2 174.2(2) . . ? C1 Sm1 Si2 125.6(2) . . ? C9 Sm1 Si2 148.1(2) . . ? N3 Sm1 Si4 31.67(16) . . ? N2 Sm1 Si4 116.71(16) . . ? N1 Sm1 Si4 104.01(15) . . ? C3 Sm1 Si4 106.0(2) . . ? C2 Sm1 Si4 135.3(2) . . ? C4 Sm1 Si4 91.5(2) . . ? C1 Sm1 Si4 138.4(2) . . ? C9 Sm1 Si4 108.7(2) . . ? Si2 Sm1 Si4 93.71(7) . . ? N3 Sm1 H2 84.6(15) . . ? N2 Sm1 H2 60.5(3) . . ? N1 Sm1 H2 66.8(14) . . ? C3 Sm1 H2 171.4(11) . . ? C2 Sm1 H2 150.8(9) . . ? C4 Sm1 H2 157.2(4) . . ? C1 Sm1 H2 135.8(15) . . ? C9 Sm1 H2 139.1(12) . . ? Si2 Sm1 H2 28.2(3) . . ? Si4 Sm1 H2 73.4(11) . . ? N2 Si1 C20 113.4(4) . . ? N2 Si1 C19 113.2(4) . . ? C20 Si1 C19 107.5(6) . . ? N2 Si1 H1 104(3) . . ? C20 Si1 H1 105(3) . . ? C19 Si1 H1 113(3) . . ? N2 Si2 C21 114.0(5) . . ? N2 Si2 C22' 116.0(17) . . ? C21 Si2 C22' 104.9(19) . . ? N2 Si2 C22 117.6(18) . . ? C21 Si2 C22 115.9(18) . . ? C22' Si2 C22 16.5(15) . . ? N2 Si2 Sm1 46.5(2) . . ? C21 Si2 Sm1 123.9(4) . . ? C22' Si2 Sm1 131.2(18) . . ? C22 Si2 Sm1 118.9(16) . . ? N2 Si2 H2 103(3) . . ? C21 Si2 H2 106(3) . . ? C22' Si2 H2 113(3) . . ? C22 Si2 H2 98(3) . . ? Sm1 Si2 H2 56(3) . . ? N3 Si3 C24 104.4(10) . . ? N3 Si3 C23 102.5(10) . . ? C24 Si3 C23 93.0(13) . . ? N3 Si3 H3 131(6) . . ? C24 Si3 H3 107(7) . . ? C23 Si3 H3 112(6) . . ? N3 Si3' C24' 119.7(11) . . ? N3 Si3' C23' 117.6(11) . . ? C24' Si3' C23' 112.9(14) . . ? N3 Si3' H3' 120(7) . . ? C24' Si3' H3' 106(7) . . ? C23' Si3' H3' 70(8) . . ? N3 Si4 C26 115.7(4) . . ? N3 Si4 C25 117.3(4) . . ? C26 Si4 C25 109.0(5) . . ? N3 Si4 Sm1 45.7(2) . . ? C26 Si4 Sm1 118.5(4) . . ? C25 Si4 Sm1 132.1(4) . . ? N3 Si4 H4 103(2) . . ? C26 Si4 H4 105(2) . . ? C25 Si4 H4 106(2) . . ? Sm1 Si4 H4 58(2) . . ? C16 N1 C12 118.9(7) . . ? C16 N1 Sm1 118.9(5) . . ? C12 N1 Sm1 121.6(5) . . ? Si2 N2 Si1 125.4(4) . . ? Si2 N2 Sm1 101.3(3) . . ? Si1 N2 Sm1 133.0(3) . . ? Si3' N3 Si4 133.0(4) . . ? Si3' N3 Si3 25.2(2) . . ? Si4 N3 Si3 124.7(4) . . ? Si3' N3 Sm1 123.4(4) . . ? Si4 N3 Sm1 102.7(3) . . ? Si3 N3 Sm1 129.2(4) . . ? C2 C1 C9 105.3(8) . . ? C2 C1 C10 125.3(9) . . ? C9 C1 C10 129.3(9) . . ? C2 C1 Sm1 73.6(5) . . ? C9 C1 Sm1 76.1(5) . . ? C10 C1 Sm1 118.2(5) . . ? C3 C2 C1 111.3(9) . . ? C3 C2 Sm1 74.3(5) . . ? C1 C2 Sm1 76.5(5) . . ? C3 C2 H2A 124.0 . . ? C1 C2 H2A 124.0 . . ? Sm1 C2 H2A 124.0 . . ? C2 C3 C4 108.5(9) . . ? C2 C3 Sm1 76.3(5) . . ? C4 C3 Sm1 77.0(6) . . ? C2 C3 H3A 124.9 . . ? C4 C3 H3A 124.9 . . ? Sm1 C3 H3A 124.9 . . ? C3 C4 C5 133.8(9) . . ? C3 C4 C9 107.5(8) . . ? C5 C4 C9 118.7(9) . . ? C3 C4 Sm1 73.4(5) . . ? C5 C4 Sm1 115.3(6) . . ? C9 C4 Sm1 76.6(5) . . ? C6 C5 C4 119.2(9) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C5 C6 C7 123.7(9) . . ? C5 C6 H6 118.1 . . ? C7 C6 H6 118.1 . . ? C8 C7 C6 120.6(10) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 118.0(9) . . ? C7 C8 H8 121.0 . . ? C9 C8 H8 121.0 . . ? C8 C9 C1 132.7(9) . . ? C8 C9 C4 119.8(9) . . ? C1 C9 C4 107.3(9) . . ? C8 C9 Sm1 114.2(6) . . ? C1 C9 Sm1 73.9(5) . . ? C4 C9 Sm1 73.0(5) . . ? C1 C10 C18 111.7(7) . . ? C1 C10 C11 111.9(6) . . ? C18 C10 C11 111.1(8) . . ? C1 C10 C17 108.9(8) . . ? C18 C10 C17 107.6(7) . . ? C11 C10 C17 105.4(7) . . ? C12 C11 C10 115.9(7) . . ? C12 C11 H11A 108.3 . . ? C10 C11 H11A 108.3 . . ? C12 C11 H11B 108.3 . . ? C10 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? N1 C12 C13 120.8(9) . . ? N1 C12 C11 118.1(7) . . ? C13 C12 C11 121.1(9) . . ? C14 C13 C12 119.9(10) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 119.6(10) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C16 118.9(10) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? N1 C16 C15 121.9(9) . . ? N1 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 C18 H18A 109.5 . . ? C10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C10 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 . . ? Si2 C22 H22C 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 . . ? Si3 C23 H3' 82(3) . . ? H3' C23 H23A 143.6 . . ? H3' C23 H23B 98.3 . . ? H3' C23 H23C 36.7 . . ? Si3' C23' H23D 109.5 . . ? Si3' C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? Si3' C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? Si3' C24' H24D 109.5 . . ? Si3' C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? Si3' C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? Si4 C25 H25A 109.5 . . ? Si4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 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 Sm1 Si2 N2 -106.2(3) . . . . ? N1 Sm1 Si2 N2 118.6(3) . . . . ? C3 Sm1 Si2 N2 -12.3(5) . . . . ? C2 Sm1 Si2 N2 19.7(4) . . . . ? C4 Sm1 Si2 N2 16(2) . . . . ? C1 Sm1 Si2 N2 56.7(4) . . . . ? C9 Sm1 Si2 N2 86.9(5) . . . . ? Si4 Sm1 Si2 N2 -137.8(3) . . . . ? N3 Sm1 Si2 C21 161.6(4) . . . . ? N2 Sm1 Si2 C21 -92.2(5) . . . . ? N1 Sm1 Si2 C21 26.4(4) . . . . ? C3 Sm1 Si2 C21 -104.5(5) . . . . ? C2 Sm1 Si2 C21 -72.5(5) . . . . ? C4 Sm1 Si2 C21 -76(2) . . . . ? C1 Sm1 Si2 C21 -35.5(5) . . . . ? C9 Sm1 Si2 C21 -5.3(6) . . . . ? Si4 Sm1 Si2 C21 130.0(4) . . . . ? N3 Sm1 Si2 C22' -17.8(13) . . . . ? N2 Sm1 Si2 C22' 88.4(13) . . . . ? N1 Sm1 Si2 C22' -153.0(13) . . . . ? C3 Sm1 Si2 C22' 76.0(14) . . . . ? C2 Sm1 Si2 C22' 108.1(13) . . . . ? C4 Sm1 Si2 C22' 105(2) . . . . ? C1 Sm1 Si2 C22' 145.0(13) . . . . ? C9 Sm1 Si2 C22' 175.2(14) . . . . ? Si4 Sm1 Si2 C22' -49.5(13) . . . . ? N3 Sm1 Si2 C22 -4.4(13) . . . . ? N2 Sm1 Si2 C22 101.8(13) . . . . ? N1 Sm1 Si2 C22 -139.6(13) . . . . ? C3 Sm1 Si2 C22 89.5(13) . . . . ? C2 Sm1 Si2 C22 121.5(13) . . . . ? C4 Sm1 Si2 C22 118(2) . . . . ? C1 Sm1 Si2 C22 158.5(13) . . . . ? C9 Sm1 Si2 C22 -171.3(14) . . . . ? Si4 Sm1 Si2 C22 -36.0(13) . . . . ? N2 Sm1 Si4 N3 63.8(4) . . . . ? N1 Sm1 Si4 N3 167.4(3) . . . . ? C3 Sm1 Si4 N3 -63.8(4) . . . . ? C2 Sm1 Si4 N3 -66.3(4) . . . . ? C4 Sm1 Si4 N3 -90.0(4) . . . . ? C1 Sm1 Si4 N3 -110.4(5) . . . . ? C9 Sm1 Si4 N3 -115.6(4) . . . . ? Si2 Sm1 Si4 N3 87.5(3) . . . . ? N3 Sm1 Si4 C26 -99.2(5) . . . . ? N2 Sm1 Si4 C26 -35.4(5) . . . . ? N1 Sm1 Si4 C26 68.2(5) . . . . ? C3 Sm1 Si4 C26 -163.0(5) . . . . ? C2 Sm1 Si4 C26 -165.6(5) . . . . ? C4 Sm1 Si4 C26 170.8(5) . . . . ? C1 Sm1 Si4 C26 150.4(5) . . . . ? C9 Sm1 Si4 C26 145.1(5) . . . . ? Si2 Sm1 Si4 C26 -11.8(4) . . . . ? N3 Sm1 Si4 C25 88.9(6) . . . . ? N2 Sm1 Si4 C25 152.7(5) . . . . ? N1 Sm1 Si4 C25 -103.7(5) . . . . ? C3 Sm1 Si4 C25 25.1(5) . . . . ? C2 Sm1 Si4 C25 22.5(6) . . . . ? C4 Sm1 Si4 C25 -1.1(5) . . . . ? C1 Sm1 Si4 C25 -21.5(6) . . . . ? C9 Sm1 Si4 C25 -26.8(5) . . . . ? Si2 Sm1 Si4 C25 176.4(5) . . . . ? N3 Sm1 N1 C16 8.1(7) . . . . ? N2 Sm1 N1 C16 118.2(5) . . . . ? C3 Sm1 N1 C16 -120.0(5) . . . . ? C2 Sm1 N1 C16 -145.5(5) . . . . ? C4 Sm1 N1 C16 -95.7(6) . . . . ? C1 Sm1 N1 C16 -138.1(6) . . . . ? C9 Sm1 N1 C16 -106.8(6) . . . . ? Si2 Sm1 N1 C16 90.1(5) . . . . ? Si4 Sm1 N1 C16 -1.1(5) . . . . ? N3 Sm1 N1 C12 179.0(5) . . . . ? N2 Sm1 N1 C12 -71.0(6) . . . . ? C3 Sm1 N1 C12 50.8(6) . . . . ? C2 Sm1 N1 C12 25.4(6) . . . . ? C4 Sm1 N1 C12 75.1(6) . . . . ? C1 Sm1 N1 C12 32.8(5) . . . . ? C9 Sm1 N1 C12 64.1(6) . . . . ? Si2 Sm1 N1 C12 -99.1(5) . . . . ? Si4 Sm1 N1 C12 169.7(5) . . . . ? C21 Si2 N2 Si1 -70.8(6) . . . . ? C22' Si2 N2 Si1 51.3(14) . . . . ? C22 Si2 N2 Si1 69.7(11) . . . . ? Sm1 Si2 N2 Si1 174.5(6) . . . . ? C21 Si2 N2 Sm1 114.7(4) . . . . ? C22' Si2 N2 Sm1 -123.2(13) . . . . ? C22 Si2 N2 Sm1 -104.8(10) . . . . ? C20 Si1 N2 Si2 71.7(7) . . . . ? C19 Si1 N2 Si2 -51.2(7) . . . . ? C20 Si1 N2 Sm1 -115.7(6) . . . . ? C19 Si1 N2 Sm1 121.4(6) . . . . ? N3 Sm1 N2 Si2 77.2(3) . . . . ? N1 Sm1 N2 Si2 -60.1(3) . . . . ? C3 Sm1 N2 Si2 172.4(3) . . . . ? C2 Sm1 N2 Si2 -164.1(3) . . . . ? C4 Sm1 N2 Si2 -177.4(3) . . . . ? C1 Sm1 N2 Si2 -135.4(3) . . . . ? C9 Sm1 N2 Si2 -132.1(4) . . . . ? Si4 Sm1 N2 Si2 48.6(3) . . . . ? N3 Sm1 N2 Si1 -96.7(5) . . . . ? N1 Sm1 N2 Si1 126.0(5) . . . . ? C3 Sm1 N2 Si1 -1.5(6) . . . . ? C2 Sm1 N2 Si1 22.1(5) . . . . ? C4 Sm1 N2 Si1 8.8(7) . . . . ? C1 Sm1 N2 Si1 50.7(5) . . . . ? C9 Sm1 N2 Si1 54.0(6) . . . . ? Si2 Sm1 N2 Si1 -173.9(7) . . . . ? Si4 Sm1 N2 Si1 -125.3(4) . . . . ? C24' Si3' N3 Si4 -155.1(11) . . . . ? C23' Si3' N3 Si4 -11.6(13) . . . . ? C24' Si3' N3 Si3 -73.8(12) . . . . ? C23' Si3' N3 Si3 69.8(12) . . . . ? C24' Si3' N3 Sm1 38.4(12) . . . . ? C23' Si3' N3 Sm1 -178.1(11) . . . . ? C26 Si4 N3 Si3' -62.9(8) . . . . ? C25 Si4 N3 Si3' 68.1(8) . . . . ? Sm1 Si4 N3 Si3' -168.5(8) . . . . ? C26 Si4 N3 Si3 -93.6(7) . . . . ? C25 Si4 N3 Si3 37.3(7) . . . . ? Sm1 Si4 N3 Si3 160.8(7) . . . . ? C26 Si4 N3 Sm1 105.6(5) . . . . ? C25 Si4 N3 Sm1 -123.4(4) . . . . ? C24 Si3 N3 Si3' 45.8(11) . . . . ? C23 Si3 N3 Si3' -50.6(12) . . . . ? C24 Si3 N3 Si4 164.1(10) . . . . ? C23 Si3 N3 Si4 67.7(11) . . . . ? C24 Si3 N3 Sm1 -40.4(11) . . . . ? C23 Si3 N3 Sm1 -136.8(11) . . . . ? N2 Sm1 N3 Si3' 44.4(5) . . . . ? N1 Sm1 N3 Si3' 152.6(4) . . . . ? C3 Sm1 N3 Si3' -69.7(5) . . . . ? C2 Sm1 N3 Si3' -56.5(5) . . . . ? C4 Sm1 N3 Si3' -99.3(5) . . . . ? C1 Sm1 N3 Si3' -82.6(6) . . . . ? C9 Sm1 N3 Si3' -112.0(5) . . . . ? Si2 Sm1 N3 Si3' 75.8(5) . . . . ? Si4 Sm1 N3 Si3' 169.9(7) . . . . ? N2 Sm1 N3 Si4 -125.5(3) . . . . ? N1 Sm1 N3 Si4 -17.3(5) . . . . ? C3 Sm1 N3 Si4 120.4(4) . . . . ? C2 Sm1 N3 Si4 133.6(3) . . . . ? C4 Sm1 N3 Si4 90.8(4) . . . . ? C1 Sm1 N3 Si4 107.5(4) . . . . ? C9 Sm1 N3 Si4 78.0(4) . . . . ? Si2 Sm1 N3 Si4 -94.1(3) . . . . ? N2 Sm1 N3 Si3 75.0(5) . . . . ? N1 Sm1 N3 Si3 -176.8(4) . . . . ? C3 Sm1 N3 Si3 -39.1(5) . . . . ? C2 Sm1 N3 Si3 -26.0(6) . . . . ? C4 Sm1 N3 Si3 -68.8(5) . . . . ? C1 Sm1 N3 Si3 -52.1(7) . . . . ? C9 Sm1 N3 Si3 -81.5(6) . . . . ? Si2 Sm1 N3 Si3 106.4(5) . . . . ? Si4 Sm1 N3 Si3 -159.6(7) . . . . ? N3 Sm1 C1 C2 51.9(7) . . . . ? N2 Sm1 C1 C2 -73.8(6) . . . . ? N1 Sm1 C1 C2 -165.4(6) . . . . ? C3 Sm1 C1 C2 34.8(5) . . . . ? C4 Sm1 C1 C2 73.8(6) . . . . ? C9 Sm1 C1 C2 110.8(8) . . . . ? Si2 Sm1 C1 C2 -101.3(5) . . . . ? Si4 Sm1 C1 C2 100.9(6) . . . . ? N3 Sm1 C1 C9 -59.0(7) . . . . ? N2 Sm1 C1 C9 175.4(5) . . . . ? N1 Sm1 C1 C9 83.7(6) . . . . ? C3 Sm1 C1 C9 -76.0(6) . . . . ? C2 Sm1 C1 C9 -110.8(8) . . . . ? C4 Sm1 C1 C9 -37.0(5) . . . . ? Si2 Sm1 C1 C9 147.9(5) . . . . ? Si4 Sm1 C1 C9 -10.0(7) . . . . ? N3 Sm1 C1 C10 173.6(6) . . . . ? N2 Sm1 C1 C10 48.0(7) . . . . ? N1 Sm1 C1 C10 -43.7(7) . . . . ? C3 Sm1 C1 C10 156.6(8) . . . . ? C2 Sm1 C1 C10 121.8(10) . . . . ? C4 Sm1 C1 C10 -164.4(9) . . . . ? C9 Sm1 C1 C10 -127.4(10) . . . . ? Si2 Sm1 C1 C10 20.5(8) . . . . ? Si4 Sm1 C1 C10 -137.4(5) . . . . ? C9 C1 C2 C3 3.2(10) . . . . ? C10 C1 C2 C3 179.8(8) . . . . ? Sm1 C1 C2 C3 -66.9(6) . . . . ? C9 C1 C2 Sm1 70.1(6) . . . . ? C10 C1 C2 Sm1 -113.3(8) . . . . ? N3 Sm1 C2 C3 -27.7(7) . . . . ? N2 Sm1 C2 C3 -131.7(6) . . . . ? N1 Sm1 C2 C3 131.5(6) . . . . ? C4 Sm1 C2 C3 37.4(5) . . . . ? C1 Sm1 C2 C3 117.1(8) . . . . ? C9 Sm1 C2 C3 78.4(6) . . . . ? Si2 Sm1 C2 C3 -142.2(5) . . . . ? Si4 Sm1 C2 C3 5.0(7) . . . . ? N3 Sm1 C2 C1 -144.8(5) . . . . ? N2 Sm1 C2 C1 111.2(5) . . . . ? N1 Sm1 C2 C1 14.4(6) . . . . ? C3 Sm1 C2 C1 -117.1(8) . . . . ? C4 Sm1 C2 C1 -79.7(6) . . . . ? C9 Sm1 C2 C1 -38.6(5) . . . . ? Si2 Sm1 C2 C1 100.8(5) . . . . ? Si4 Sm1 C2 C1 -112.0(5) . . . . ? C1 C2 C3 C4 -2.6(10) . . . . ? Sm1 C2 C3 C4 -70.9(6) . . . . ? C1 C2 C3 Sm1 68.3(6) . . . . ? N3 Sm1 C3 C2 155.6(6) . . . . ? N2 Sm1 C3 C2 54.2(6) . . . . ? N1 Sm1 C3 C2 -58.4(6) . . . . ? C4 Sm1 C3 C2 -113.1(8) . . . . ? C1 Sm1 C3 C2 -35.4(5) . . . . ? C9 Sm1 C3 C2 -75.2(6) . . . . ? Si2 Sm1 C3 C2 61.3(7) . . . . ? Si4 Sm1 C3 C2 -176.3(5) . . . . ? N3 Sm1 C3 C4 -91.4(5) . . . . ? N2 Sm1 C3 C4 167.3(5) . . . . ? N1 Sm1 C3 C4 54.6(6) . . . . ? C2 Sm1 C3 C4 113.1(8) . . . . ? C1 Sm1 C3 C4 77.6(6) . . . . ? C9 Sm1 C3 C4 37.8(5) . . . . ? Si2 Sm1 C3 C4 174.4(4) . . . . ? Si4 Sm1 C3 C4 -63.3(5) . . . . ? C2 C3 C4 C5 179.9(9) . . . . ? Sm1 C3 C4 C5 109.4(10) . . . . ? C2 C3 C4 C9 0.9(10) . . . . ? Sm1 C3 C4 C9 -69.6(6) . . . . ? C2 C3 C4 Sm1 70.5(6) . . . . ? N3 Sm1 C4 C3 89.2(5) . . . . ? N2 Sm1 C4 C3 -19.2(7) . . . . ? N1 Sm1 C4 C3 -134.5(5) . . . . ? C2 Sm1 C4 C3 -37.0(5) . . . . ? C1 Sm1 C4 C3 -76.7(6) . . . . ? C9 Sm1 C4 C3 -113.2(8) . . . . ? Si2 Sm1 C4 C3 -33(2) . . . . ? Si4 Sm1 C4 C3 120.8(5) . . . . ? N3 Sm1 C4 C5 -42.0(7) . . . . ? N2 Sm1 C4 C5 -150.4(6) . . . . ? N1 Sm1 C4 C5 94.3(7) . . . . ? C3 Sm1 C4 C5 -131.1(10) . . . . ? C2 Sm1 C4 C5 -168.2(9) . . . . ? C1 Sm1 C4 C5 152.1(9) . . . . ? C9 Sm1 C4 C5 115.7(10) . . . . ? Si2 Sm1 C4 C5 -164.4(16) . . . . ? Si4 Sm1 C4 C5 -10.3(7) . . . . ? N3 Sm1 C4 C9 -157.6(6) . . . . ? N2 Sm1 C4 C9 94.0(7) . . . . ? N1 Sm1 C4 C9 -21.3(6) . . . . ? C3 Sm1 C4 C9 113.2(8) . . . . ? C2 Sm1 C4 C9 76.2(6) . . . . ? C1 Sm1 C4 C9 36.5(5) . . . . ? Si2 Sm1 C4 C9 80(2) . . . . ? Si4 Sm1 C4 C9 -126.0(5) . . . . ? C3 C4 C5 C6 -177.0(9) . . . . ? C9 C4 C5 C6 1.9(12) . . . . ? Sm1 C4 C5 C6 -86.1(9) . . . . ? C4 C5 C6 C7 -0.2(13) . . . . ? C5 C6 C7 C8 -0.4(13) . . . . ? C6 C7 C8 C9 -0.9(12) . . . . ? C7 C8 C9 C1 176.1(9) . . . . ? C7 C8 C9 C4 2.6(12) . . . . ? C7 C8 C9 Sm1 86.1(9) . . . . ? C2 C1 C9 C8 -176.6(9) . . . . ? C10 C1 C9 C8 6.9(16) . . . . ? Sm1 C1 C9 C8 -108.3(10) . . . . ? C2 C1 C9 C4 -2.5(9) . . . . ? C10 C1 C9 C4 -179.0(8) . . . . ? Sm1 C1 C9 C4 65.8(6) . . . . ? C2 C1 C9 Sm1 -68.3(6) . . . . ? C10 C1 C9 Sm1 115.2(9) . . . . ? C3 C4 C9 C8 176.1(8) . . . . ? C5 C4 C9 C8 -3.1(12) . . . . ? Sm1 C4 C9 C8 108.6(8) . . . . ? C3 C4 C9 C1 1.1(10) . . . . ? C5 C4 C9 C1 -178.1(8) . . . . ? Sm1 C4 C9 C1 -66.4(6) . . . . ? C3 C4 C9 Sm1 67.5(6) . . . . ? C5 C4 C9 Sm1 -111.7(8) . . . . ? N3 Sm1 C9 C8 -89.8(7) . . . . ? N2 Sm1 C9 C8 123.7(6) . . . . ? N1 Sm1 C9 C8 42.6(6) . . . . ? C3 Sm1 C9 C8 -152.3(8) . . . . ? C2 Sm1 C9 C8 168.4(8) . . . . ? C4 Sm1 C9 C8 -115.6(9) . . . . ? C1 Sm1 C9 C8 130.0(10) . . . . ? Si2 Sm1 C9 C8 75.3(8) . . . . ? Si4 Sm1 C9 C8 -56.9(7) . . . . ? N3 Sm1 C9 C1 140.2(5) . . . . ? N2 Sm1 C9 C1 -6.3(7) . . . . ? N1 Sm1 C9 C1 -87.4(6) . . . . ? C3 Sm1 C9 C1 77.6(6) . . . . ? C2 Sm1 C9 C1 38.4(5) . . . . ? C4 Sm1 C9 C1 114.4(9) . . . . ? Si2 Sm1 C9 C1 -54.8(8) . . . . ? Si4 Sm1 C9 C1 173.0(5) . . . . ? N3 Sm1 C9 C4 25.8(6) . . . . ? N2 Sm1 C9 C4 -120.7(5) . . . . ? N1 Sm1 C9 C4 158.2(6) . . . . ? C3 Sm1 C9 C4 -36.7(5) . . . . ? C2 Sm1 C9 C4 -76.0(6) . . . . ? C1 Sm1 C9 C4 -114.4(9) . . . . ? Si2 Sm1 C9 C4 -169.2(4) . . . . ? Si4 Sm1 C9 C4 58.7(6) . . . . ? C2 C1 C10 C18 -136.3(9) . . . . ? C9 C1 C10 C18 39.5(12) . . . . ? Sm1 C1 C10 C18 134.4(6) . . . . ? C2 C1 C10 C11 98.5(10) . . . . ? C9 C1 C10 C11 -85.7(11) . . . . ? Sm1 C1 C10 C11 9.2(10) . . . . ? C2 C1 C10 C17 -17.7(12) . . . . ? C9 C1 C10 C17 158.1(9) . . . . ? Sm1 C1 C10 C17 -106.9(7) . . . . ? C1 C10 C11 C12 64.6(10) . . . . ? C18 C10 C11 C12 -61.0(9) . . . . ? C17 C10 C11 C12 -177.2(7) . . . . ? C16 N1 C12 C13 1.0(11) . . . . ? Sm1 N1 C12 C13 -169.8(6) . . . . ? C16 N1 C12 C11 -176.2(7) . . . . ? Sm1 N1 C12 C11 13.0(9) . . . . ? C10 C11 C12 N1 -84.3(9) . . . . ? C10 C11 C12 C13 98.6(10) . . . . ? N1 C12 C13 C14 0.3(14) . . . . ? C11 C12 C13 C14 177.4(9) . . . . ? C12 C13 C14 C15 -1.1(15) . . . . ? C13 C14 C15 C16 0.6(15) . . . . ? C12 N1 C16 C15 -1.6(11) . . . . ? Sm1 N1 C16 C15 169.5(6) . . . . ? C14 C15 C16 N1 0.8(13) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.414 _refine_diff_density_min -1.467 _refine_diff_density_rms 0.127 data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 900282' #TrackingRef 'CCDC 900280.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H46 Er N3 Si4' _chemical_formula_sum 'C26 H46 Er N3 Si4' _chemical_formula_weight 680.28 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.3771(17) _cell_length_b 8.3270(7) _cell_length_c 22.582(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.130(3) _cell_angle_gamma 90.00 _cell_volume 3265.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7928 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 2.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.291 _exptl_absorpt_correction_T_max 0.593 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16198 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6029 _reflns_number_gt 5316 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+6.2277P] 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 6029 _refine_ls_number_parameters 304 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1098 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.736575(15) 0.26896(3) 0.850877(12) 0.03891(11) Uani 1 1 d . A . Si1 Si 0.91967(10) 0.3237(2) 0.93181(9) 0.0507(5) Uani 1 1 d D . . H1 H 0.897(3) 0.492(3) 0.920(3) 0.07(2) Uiso 1 1 d D . . Si2 Si 0.83173(12) 0.0160(2) 0.91623(10) 0.0600(6) Uani 1 1 d D . . H2 H 0.7525(15) 0.002(8) 0.890(3) 0.07(2) Uiso 1 1 d D . . Si3 Si 0.6421(2) 0.4150(6) 0.9804(2) 0.0604(8) Uiso 0.50 1 d PD A 1 H3 H 0.610(4) 0.578(4) 0.971(4) 0.01(2) Uiso 0.50 1 d PD B 1 Si3' Si 0.6721(2) 0.3502(6) 0.9945(2) 0.0604(8) Uiso 0.50 1 d PD A 2 H3' H 0.694(8) 0.226(12) 1.039(4) 0.07(4) Uiso 0.50 1 d PD C 2 Si4 Si 0.58510(11) 0.1510(3) 0.89871(10) 0.0570(5) Uani 1 1 d D A . H4 H 0.609(3) 0.133(6) 0.8368(9) 0.040(15) Uiso 1 1 d D . . N1 N 0.7574(3) 0.0734(6) 0.7682(2) 0.0504(14) Uani 1 1 d . . . N2 N 0.8451(3) 0.2139(6) 0.9026(2) 0.0432(12) Uani 1 1 d . . . N3 N 0.6542(3) 0.2741(6) 0.9248(3) 0.0504(14) Uani 1 1 d . . . C1 C 0.7830(4) 0.4520(8) 0.7617(3) 0.0516(17) Uani 1 1 d . . . C2 C 0.7923(4) 0.5418(8) 0.8141(3) 0.0596(19) Uani 1 1 d . A . H2A H 0.8420 0.5877 0.8287 0.072 Uiso 1 1 calc R . . C3 C 0.7215(5) 0.5798(8) 0.8374(3) 0.066(2) Uani 1 1 d . . . H3A H 0.7130 0.6582 0.8694 0.079 Uiso 1 1 calc R A . C4 C 0.6651(4) 0.5175(10) 0.7989(4) 0.0698(9) Uani 1 1 d . A . C5 C 0.5831(4) 0.5211(10) 0.7985(4) 0.0698(9) Uani 1 1 d . . . H5 H 0.5574 0.5731 0.8289 0.084 Uiso 1 1 calc R A . C6 C 0.5423(4) 0.4475(10) 0.7530(4) 0.0698(9) Uani 1 1 d . A . H6 H 0.4882 0.4531 0.7521 0.084 Uiso 1 1 calc R . . C7 C 0.5783(4) 0.3647(10) 0.7082(4) 0.0698(9) Uani 1 1 d . . . H7 H 0.5478 0.3124 0.6788 0.084 Uiso 1 1 calc R A . C8 C 0.6561(4) 0.3572(10) 0.7056(4) 0.0698(9) Uani 1 1 d . A . H8 H 0.6793 0.3019 0.6747 0.084 Uiso 1 1 calc R . . C9 C 0.7020(4) 0.4350(10) 0.7508(4) 0.0698(9) Uani 1 1 d . A . C10 C 0.8505(4) 0.3966(10) 0.7256(4) 0.064(2) Uani 1 1 d . A . C11 C 0.8734(4) 0.2222(10) 0.7421(4) 0.068(2) Uani 1 1 d . . . H11A H 0.9200 0.1951 0.7212 0.082 Uiso 1 1 calc R A . H11B H 0.8867 0.2193 0.7846 0.082 Uiso 1 1 calc R . . C12 C 0.8144(4) 0.0929(9) 0.7290(3) 0.0584(19) Uani 1 1 d . A . C13 C 0.8180(6) -0.0039(11) 0.6806(4) 0.087(3) Uani 1 1 d . . . H13 H 0.8580 0.0103 0.6542 0.104 Uiso 1 1 calc R A . C14 C 0.7644(7) -0.1216(11) 0.6698(4) 0.098(3) Uani 1 1 d . A . H14 H 0.7661 -0.1853 0.6356 0.118 Uiso 1 1 calc R . . C15 C 0.7082(6) -0.1449(9) 0.7100(4) 0.079(2) Uani 1 1 d . . . H15 H 0.6711 -0.2263 0.7044 0.094 Uiso 1 1 calc R A . C16 C 0.7077(4) -0.0468(8) 0.7580(3) 0.0555(18) Uani 1 1 d . A . H16 H 0.6699 -0.0647 0.7860 0.067 Uiso 1 1 calc R . . C17 C 0.9223(5) 0.5015(12) 0.7406(5) 0.096(3) Uani 1 1 d . . . H17A H 0.9101 0.6134 0.7327 0.145 Uiso 1 1 calc R A . H17B H 0.9644 0.4683 0.7164 0.145 Uiso 1 1 calc R . . H17C H 0.9372 0.4886 0.7821 0.145 Uiso 1 1 calc R . . C18 C 0.8316(5) 0.4099(11) 0.6585(3) 0.081(3) Uani 1 1 d . . . H18A H 0.7910 0.3345 0.6474 0.121 Uiso 1 1 calc R A . H18B H 0.8772 0.3854 0.6367 0.121 Uiso 1 1 calc R . . H18C H 0.8146 0.5182 0.6491 0.121 Uiso 1 1 calc R . . C19 C 0.9370(6) 0.2942(12) 1.0123(4) 0.096(3) Uani 1 1 d . . . H19A H 0.8918 0.3273 1.0331 0.144 Uiso 1 1 calc R . . H19B H 0.9809 0.3581 1.0257 0.144 Uiso 1 1 calc R . . H19C H 0.9474 0.1816 1.0202 0.144 Uiso 1 1 calc R . . C20 C 1.0130(5) 0.2795(13) 0.8967(5) 0.109(4) Uani 1 1 d . . . H20A H 1.0233 0.1652 0.8989 0.164 Uiso 1 1 calc R . . H20B H 1.0541 0.3376 0.9175 0.164 Uiso 1 1 calc R . . H20C H 1.0099 0.3129 0.8556 0.164 Uiso 1 1 calc R . . C21 C 0.9033(5) -0.1167(10) 0.8814(5) 0.105(4) Uani 1 1 d . . . H21A H 0.8981 -0.1071 0.8386 0.158 Uiso 1 1 calc R . . H21B H 0.8942 -0.2272 0.8928 0.158 Uiso 1 1 calc R . . H21C H 0.9548 -0.0851 0.8946 0.158 Uiso 1 1 calc R . . C22 C 0.8190(7) -0.0459(12) 0.9943(5) 0.128(5) Uani 1 1 d . . . H22A H 0.8678 -0.0371 1.0163 0.193 Uiso 1 1 calc R . . H22B H 0.8012 -0.1563 0.9952 0.193 Uiso 1 1 calc R . . H22C H 0.7813 0.0233 1.0120 0.193 Uiso 1 1 calc R . . C23 C 0.6127(12) 0.296(2) 1.0485(9) 0.088(4) Uiso 0.50 1 d PD A 1 H23A H 0.5572 0.2833 1.0477 0.132 Uiso 0.50 1 calc PR A 1 H23B H 0.6293 0.3528 1.0842 0.132 Uiso 0.50 1 calc PR A 1 H23C H 0.6368 0.1907 1.0482 0.132 Uiso 0.50 1 calc PR A 1 C23' C 0.5896(10) 0.344(3) 1.0448(9) 0.088(4) Uiso 0.50 1 d PD A 2 H23D H 0.5431 0.3783 1.0233 0.132 Uiso 0.50 1 calc PR A 2 H23E H 0.5998 0.4154 1.0781 0.132 Uiso 0.50 1 calc PR A 2 H23F H 0.5829 0.2353 1.0591 0.132 Uiso 0.50 1 calc PR A 2 C24 C 0.7424(9) 0.470(2) 1.0089(10) 0.097(5) Uiso 0.50 1 d PD A 1 H24A H 0.7696 0.3740 1.0217 0.146 Uiso 0.50 1 calc PR A 1 H24B H 0.7389 0.5437 1.0421 0.146 Uiso 0.50 1 calc PR A 1 H24C H 0.7700 0.5217 0.9775 0.146 Uiso 0.50 1 calc PR A 1 C24' C 0.7190(11) 0.5483(19) 0.9989(10) 0.097(5) Uiso 0.50 1 d PD A 2 H24D H 0.7282 0.5868 0.9593 0.146 Uiso 0.50 1 calc PR A 2 H24E H 0.7676 0.5391 1.0211 0.146 Uiso 0.50 1 calc PR A 2 H24F H 0.6859 0.6234 1.0187 0.146 Uiso 0.50 1 calc PR A 2 C25 C 0.4842(4) 0.2279(10) 0.8932(5) 0.081(3) Uani 1 1 d . . . H25A H 0.4647 0.2402 0.9326 0.121 Uiso 1 1 calc R A . H25B H 0.4521 0.1524 0.8708 0.121 Uiso 1 1 calc R . . H25C H 0.4833 0.3311 0.8732 0.121 Uiso 1 1 calc R . . C26 C 0.5841(5) -0.0531(10) 0.9322(4) 0.083(3) Uani 1 1 d . . . H26A H 0.6350 -0.1004 0.9306 0.124 Uiso 1 1 calc R A . H26B H 0.5473 -0.1200 0.9103 0.124 Uiso 1 1 calc R . . H26C H 0.5696 -0.0454 0.9731 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 0.04375(17) 0.03873(18) 0.03396(18) 0.00341(12) -0.00265(12) -0.00449(11) Si1 0.0486(10) 0.0490(11) 0.0535(12) -0.0009(9) -0.0102(9) -0.0097(8) Si2 0.0716(12) 0.0446(11) 0.0615(14) 0.0102(10) -0.0288(11) -0.0133(9) Si4 0.0521(10) 0.0604(13) 0.0589(13) -0.0028(10) 0.0073(10) -0.0098(9) N1 0.059(3) 0.045(3) 0.046(3) -0.001(3) -0.009(3) 0.006(3) N2 0.046(3) 0.042(3) 0.041(3) 0.003(2) -0.009(2) -0.008(2) N3 0.049(3) 0.059(4) 0.043(3) 0.003(3) 0.007(3) -0.011(3) C1 0.059(4) 0.056(4) 0.040(4) 0.002(3) 0.001(3) -0.008(3) C2 0.078(5) 0.046(4) 0.055(5) 0.016(3) 0.002(4) -0.016(4) C3 0.110(6) 0.035(4) 0.053(5) 0.005(3) 0.008(5) -0.001(4) C4 0.0661(18) 0.078(2) 0.065(2) 0.0245(18) -0.0070(16) 0.0052(17) C5 0.0661(18) 0.078(2) 0.065(2) 0.0245(18) -0.0070(16) 0.0052(17) C6 0.0661(18) 0.078(2) 0.065(2) 0.0245(18) -0.0070(16) 0.0052(17) C7 0.0661(18) 0.078(2) 0.065(2) 0.0245(18) -0.0070(16) 0.0052(17) C8 0.0661(18) 0.078(2) 0.065(2) 0.0245(18) -0.0070(16) 0.0052(17) C9 0.0661(18) 0.078(2) 0.065(2) 0.0245(18) -0.0070(16) 0.0052(17) C10 0.062(4) 0.071(5) 0.060(5) 0.013(4) 0.010(4) -0.005(4) C11 0.053(4) 0.094(6) 0.059(5) 0.011(4) 0.016(4) 0.011(4) C12 0.075(5) 0.058(5) 0.042(4) 0.007(3) 0.003(4) 0.017(4) C13 0.119(7) 0.071(6) 0.072(6) -0.009(5) 0.023(6) 0.015(6) C14 0.183(11) 0.059(6) 0.052(6) -0.010(5) 0.002(7) 0.022(6) C15 0.128(7) 0.046(5) 0.060(5) 0.003(4) -0.023(5) 0.001(5) C16 0.082(5) 0.038(4) 0.045(4) -0.003(3) -0.016(4) 0.006(3) C17 0.069(5) 0.110(8) 0.111(8) 0.019(6) 0.011(5) -0.025(5) C18 0.106(6) 0.094(6) 0.043(5) 0.013(4) 0.013(5) 0.006(5) C19 0.109(7) 0.114(8) 0.062(6) 0.003(5) -0.028(5) -0.057(6) C20 0.055(5) 0.142(10) 0.132(10) -0.035(7) 0.018(6) -0.028(5) C21 0.087(6) 0.051(5) 0.173(11) -0.005(6) -0.054(7) 0.012(4) C22 0.196(11) 0.094(8) 0.091(8) 0.047(6) -0.057(8) -0.077(8) C25 0.051(4) 0.097(7) 0.095(7) 0.005(5) 0.005(4) -0.007(4) C26 0.073(5) 0.070(6) 0.105(8) 0.005(5) 0.011(5) -0.023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 N2 2.229(5) . ? Er1 N3 2.240(5) . ? Er1 N1 2.513(6) . ? Er1 C2 2.617(6) . ? Er1 C3 2.618(7) . ? Er1 C4 2.664(8) . ? Er1 C1 2.674(7) . ? Er1 C9 2.699(8) . ? Er1 Si2 3.028(2) . ? Er1 Si4 3.0448(19) . ? Er1 H2 2.41(7) . ? Er1 H4 2.49(5) . ? Si1 N2 1.699(5) . ? Si1 C19 1.847(9) . ? Si1 C20 1.867(9) . ? Si1 H1 1.478(10) . ? Si2 N2 1.694(5) . ? Si2 C22 1.857(10) . ? Si2 C21 1.859(9) . ? Si2 H2 1.480(10) . ? Si3 N3 1.737(7) . ? Si3 C24 1.892(14) . ? Si3 C23 1.917(15) . ? Si3 H3 1.478(10) . ? Si3' N3 1.714(7) . ? Si3' C24' 1.841(14) . ? Si3' C23' 1.863(14) . ? Si3' H3' 1.480(10) . ? Si4 N3 1.670(6) . ? Si4 C26 1.861(8) . ? Si4 C25 1.867(8) . ? Si4 H4 1.483(10) . ? N1 C16 1.336(8) . ? N1 C12 1.364(9) . ? C1 C2 1.404(10) . ? C1 C9 1.428(9) . ? C1 C10 1.525(10) . ? C2 C3 1.393(10) . ? C2 H2A 0.9900 . ? C3 C4 1.386(11) . ? C3 H3A 0.9900 . ? C4 C5 1.425(10) . ? C4 C9 1.455(12) . ? C5 C6 1.370(11) . ? C5 H5 0.9400 . ? C6 C7 1.393(11) . ? C6 H6 0.9400 . ? C7 C8 1.357(10) . ? C7 H7 0.9400 . ? C8 C9 1.426(11) . ? C8 H8 0.9400 . ? C10 C18 1.543(11) . ? C10 C11 1.547(10) . ? C10 C17 1.549(11) . ? C11 C12 1.508(10) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.361(11) . ? C13 C14 1.368(13) . ? C13 H13 0.9400 . ? C14 C15 1.371(12) . ? C14 H14 0.9400 . ? C15 C16 1.359(10) . ? C15 H15 0.9400 . ? C16 H16 0.9400 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H3' 1.54(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C23' H23D 0.9700 . ? C23' H23E 0.9700 . ? C23' H23F 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C24' H24D 0.9700 . ? C24' H24E 0.9700 . ? C24' H24F 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Er1 N3 99.5(2) . . ? N2 Er1 N1 96.54(18) . . ? N3 Er1 N1 132.81(19) . . ? N2 Er1 C2 91.7(2) . . ? N3 Er1 C2 118.3(2) . . ? N1 Er1 C2 105.2(2) . . ? N2 Er1 C3 110.1(2) . . ? N3 Er1 C3 90.2(2) . . ? N1 Er1 C3 124.8(2) . . ? C2 Er1 C3 30.9(2) . . ? N2 Er1 C4 139.7(2) . . ? N3 Er1 C4 90.7(2) . . ? N1 Er1 C4 104.7(2) . . ? C2 Er1 C4 50.0(2) . . ? C3 Er1 C4 30.4(2) . . ? N2 Er1 C1 103.81(19) . . ? N3 Er1 C1 140.3(2) . . ? N1 Er1 C1 75.8(2) . . ? C2 Er1 C1 30.7(2) . . ? C3 Er1 C1 51.7(2) . . ? C4 Er1 C1 51.3(2) . . ? N2 Er1 C9 134.6(2) . . ? N3 Er1 C9 119.1(2) . . ? N1 Er1 C9 75.1(2) . . ? C2 Er1 C9 50.4(2) . . ? C3 Er1 C9 51.5(3) . . ? C4 Er1 C9 31.5(2) . . ? C1 Er1 C9 30.8(2) . . ? N2 Er1 Si2 33.42(13) . . ? N3 Er1 Si2 90.15(15) . . ? N1 Er1 Si2 79.64(13) . . ? C2 Er1 Si2 123.84(18) . . ? C3 Er1 Si2 142.66(19) . . ? C4 Er1 Si2 173.0(2) . . ? C1 Er1 Si2 126.07(15) . . ? C9 Er1 Si2 149.92(18) . . ? N2 Er1 Si4 118.26(14) . . ? N3 Er1 Si4 32.52(15) . . ? N1 Er1 Si4 101.80(14) . . ? C2 Er1 Si4 136.69(18) . . ? C3 Er1 Si4 106.02(18) . . ? C4 Er1 Si4 90.67(17) . . ? C1 Er1 Si4 137.75(15) . . ? C9 Er1 Si4 107.09(17) . . ? Si2 Er1 Si4 93.80(6) . . ? N2 Er1 H2 62.1(4) . . ? N3 Er1 H2 79.0(15) . . ? N1 Er1 H2 70.0(15) . . ? C2 Er1 H2 151.7(7) . . ? C3 Er1 H2 165.0(14) . . ? C4 Er1 H2 157.8(4) . . ? C1 Er1 H2 140.5(15) . . ? C9 Er1 H2 143.3(13) . . ? Si2 Er1 H2 28.8(4) . . ? Si4 Er1 H2 70.1(10) . . ? N2 Er1 H4 134.6(11) . . ? N3 Er1 H4 61.0(4) . . ? N1 Er1 H4 76.3(7) . . ? C2 Er1 H4 133.6(12) . . ? C3 Er1 H4 110.4(12) . . ? C4 Er1 H4 84.2(12) . . ? C1 Er1 H4 117.0(8) . . ? C9 Er1 H4 87.5(9) . . ? Si2 Er1 H4 102.3(12) . . ? Si4 Er1 H4 28.9(3) . . ? H2 Er1 H4 73.6(13) . . ? N2 Si1 C19 113.9(3) . . ? N2 Si1 C20 113.0(4) . . ? C19 Si1 C20 106.2(5) . . ? N2 Si1 H1 104(3) . . ? C19 Si1 H1 110(3) . . ? C20 Si1 H1 110(2) . . ? N2 Si2 C22 117.7(4) . . ? N2 Si2 C21 113.8(4) . . ? C22 Si2 C21 110.0(5) . . ? N2 Si2 Er1 46.43(18) . . ? C22 Si2 Er1 125.0(4) . . ? C21 Si2 Er1 124.7(4) . . ? N2 Si2 H2 98(3) . . ? C22 Si2 H2 102(3) . . ? C21 Si2 H2 114(3) . . ? Er1 Si2 H2 52(3) . . ? N3 Si3 C24 106.0(7) . . ? N3 Si3 C23 105.8(8) . . ? C24 Si3 C23 97.0(10) . . ? N3 Si3 H3 125(3) . . ? C24 Si3 H3 99(3) . . ? C23 Si3 H3 119(3) . . ? N3 Si3' C24' 116.5(8) . . ? N3 Si3' C23' 115.6(8) . . ? C24' Si3' C23' 109.9(10) . . ? N3 Si3' H3' 113(5) . . ? C24' Si3' H3' 119(5) . . ? C23' Si3' H3' 75(5) . . ? N3 Si4 C26 115.8(4) . . ? N3 Si4 C25 118.3(4) . . ? C26 Si4 C25 108.5(4) . . ? N3 Si4 Er1 46.16(19) . . ? C26 Si4 Er1 117.4(3) . . ? C25 Si4 Er1 133.5(3) . . ? N3 Si4 H4 100(2) . . ? C26 Si4 H4 107(2) . . ? C25 Si4 H4 106(2) . . ? Er1 Si4 H4 54(2) . . ? C16 N1 C12 117.3(6) . . ? C16 N1 Er1 120.2(5) . . ? C12 N1 Er1 122.2(5) . . ? Si2 N2 Si1 124.1(3) . . ? Si2 N2 Er1 100.1(2) . . ? Si1 N2 Er1 135.3(3) . . ? Si4 N3 Si3' 130.9(3) . . ? Si4 N3 Si3 124.4(3) . . ? Si3' N3 Si3 27.06(19) . . ? Si4 N3 Er1 101.3(3) . . ? Si3' N3 Er1 126.3(3) . . ? Si3 N3 Er1 130.5(3) . . ? C2 C1 C9 106.3(7) . . ? C2 C1 C10 123.1(6) . . ? C9 C1 C10 130.6(7) . . ? C2 C1 Er1 72.4(4) . . ? C9 C1 Er1 75.5(4) . . ? C10 C1 Er1 119.3(5) . . ? C3 C2 C1 111.4(7) . . ? C3 C2 Er1 74.6(4) . . ? C1 C2 Er1 76.9(4) . . ? C3 C2 H2A 123.9 . . ? C1 C2 H2A 123.9 . . ? Er1 C2 H2A 123.9 . . ? C4 C3 C2 107.0(7) . . ? C4 C3 Er1 76.6(4) . . ? C2 C3 Er1 74.5(4) . . ? C4 C3 H3A 125.7 . . ? C2 C3 H3A 125.7 . . ? Er1 C3 H3A 125.7 . . ? C3 C4 C5 132.9(9) . . ? C3 C4 C9 108.9(7) . . ? C5 C4 C9 118.2(8) . . ? C3 C4 Er1 73.0(4) . . ? C5 C4 Er1 118.0(5) . . ? C9 C4 Er1 75.6(4) . . ? C6 C5 C4 119.1(8) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C7 122.2(8) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C8 C7 C6 121.9(9) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C7 C8 C9 118.7(8) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C8 C9 C1 133.6(8) . . ? C8 C9 C4 119.9(7) . . ? C1 C9 C4 106.4(7) . . ? C8 C9 Er1 117.9(5) . . ? C1 C9 Er1 73.7(4) . . ? C4 C9 Er1 72.9(4) . . ? C1 C10 C18 111.3(6) . . ? C1 C10 C11 110.5(6) . . ? C18 C10 C11 110.4(7) . . ? C1 C10 C17 109.9(7) . . ? C18 C10 C17 108.4(7) . . ? C11 C10 C17 106.2(7) . . ? C12 C11 C10 117.2(6) . . ? C12 C11 H11A 108.0 . . ? C10 C11 H11A 108.0 . . ? C12 C11 H11B 108.0 . . ? C10 C11 H11B 108.0 . . ? H11A C11 H11B 107.2 . . ? C13 C12 N1 120.5(8) . . ? C13 C12 C11 122.0(8) . . ? N1 C12 C11 117.5(6) . . ? C12 C13 C14 121.0(9) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C15 118.8(8) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C16 C15 C14 117.9(9) . . ? C16 C15 H15 121.0 . . ? C14 C15 H15 121.0 . . ? N1 C16 C15 124.4(8) . . ? N1 C16 H16 117.8 . . ? C15 C16 H16 117.8 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 C18 H18A 109.5 . . ? C10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C10 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 . . ? Si3 C23 H3' 79(2) . . ? H3' C23 H23A 150.2 . . ? H3' C23 H23B 93.2 . . ? H3' C23 H23C 42.6 . . ? Si3' C23' H23D 109.5 . . ? Si3' C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? Si3' C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? Si3' C24' H24D 109.5 . . ? Si3' C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? Si3' C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? Si4 C25 H25A 109.5 . . ? Si4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 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 Si2 N2 -107.2(3) . . . . ? N1 Er1 Si2 N2 119.2(3) . . . . ? C2 Er1 Si2 N2 17.8(3) . . . . ? C3 Er1 Si2 N2 -16.6(4) . . . . ? C4 Er1 Si2 N2 -9.9(16) . . . . ? C1 Er1 Si2 N2 55.4(3) . . . . ? C9 Er1 Si2 N2 85.9(4) . . . . ? Si4 Er1 Si2 N2 -139.5(3) . . . . ? N2 Er1 Si2 C22 96.7(4) . . . . ? N3 Er1 Si2 C22 -10.5(4) . . . . ? N1 Er1 Si2 C22 -144.2(4) . . . . ? C2 Er1 Si2 C22 114.4(4) . . . . ? C3 Er1 Si2 C22 80.0(5) . . . . ? C4 Er1 Si2 C22 86.8(16) . . . . ? C1 Er1 Si2 C22 152.1(4) . . . . ? C9 Er1 Si2 C22 -177.5(5) . . . . ? Si4 Er1 Si2 C22 -42.9(4) . . . . ? N2 Er1 Si2 C21 -91.1(4) . . . . ? N3 Er1 Si2 C21 161.7(4) . . . . ? N1 Er1 Si2 C21 28.1(4) . . . . ? C2 Er1 Si2 C21 -73.3(4) . . . . ? C3 Er1 Si2 C21 -107.7(4) . . . . ? C4 Er1 Si2 C21 -100.9(16) . . . . ? C1 Er1 Si2 C21 -35.7(4) . . . . ? C9 Er1 Si2 C21 -5.2(5) . . . . ? Si4 Er1 Si2 C21 129.4(3) . . . . ? N2 Er1 Si4 N3 60.4(3) . . . . ? N1 Er1 Si4 N3 164.5(3) . . . . ? C2 Er1 Si4 N3 -67.8(4) . . . . ? C3 Er1 Si4 N3 -63.7(3) . . . . ? C4 Er1 Si4 N3 -90.3(3) . . . . ? C1 Er1 Si4 N3 -113.8(4) . . . . ? C9 Er1 Si4 N3 -117.6(3) . . . . ? Si2 Er1 Si4 N3 84.3(3) . . . . ? N2 Er1 Si4 C26 -40.1(4) . . . . ? N3 Er1 Si4 C26 -100.5(4) . . . . ? N1 Er1 Si4 C26 64.0(4) . . . . ? C2 Er1 Si4 C26 -168.3(4) . . . . ? C3 Er1 Si4 C26 -164.2(4) . . . . ? C4 Er1 Si4 C26 169.2(4) . . . . ? C1 Er1 Si4 C26 145.8(4) . . . . ? C9 Er1 Si4 C26 141.9(4) . . . . ? Si2 Er1 Si4 C26 -16.2(4) . . . . ? N2 Er1 Si4 C25 150.1(5) . . . . ? N3 Er1 Si4 C25 89.8(5) . . . . ? N1 Er1 Si4 C25 -105.7(5) . . . . ? C2 Er1 Si4 C25 22.0(5) . . . . ? C3 Er1 Si4 C25 26.1(5) . . . . ? C4 Er1 Si4 C25 -0.5(5) . . . . ? C1 Er1 Si4 C25 -24.0(5) . . . . ? C9 Er1 Si4 C25 -27.8(5) . . . . ? Si2 Er1 Si4 C25 174.1(4) . . . . ? N2 Er1 N1 C16 118.3(5) . . . . ? N3 Er1 N1 C16 8.9(6) . . . . ? C2 Er1 N1 C16 -148.1(5) . . . . ? C3 Er1 N1 C16 -121.6(5) . . . . ? C4 Er1 N1 C16 -96.2(5) . . . . ? C1 Er1 N1 C16 -139.0(5) . . . . ? C9 Er1 N1 C16 -107.2(5) . . . . ? Si2 Er1 N1 C16 89.4(5) . . . . ? Si4 Er1 N1 C16 -2.4(5) . . . . ? N2 Er1 N1 C12 -67.8(5) . . . . ? N3 Er1 N1 C12 -177.2(4) . . . . ? C2 Er1 N1 C12 25.7(5) . . . . ? C3 Er1 N1 C12 52.2(6) . . . . ? C4 Er1 N1 C12 77.6(5) . . . . ? C1 Er1 N1 C12 34.8(5) . . . . ? C9 Er1 N1 C12 66.7(5) . . . . ? Si2 Er1 N1 C12 -96.8(5) . . . . ? Si4 Er1 N1 C12 171.5(5) . . . . ? C22 Si2 N2 Si1 60.3(6) . . . . ? C21 Si2 N2 Si1 -70.4(5) . . . . ? Er1 Si2 N2 Si1 173.6(5) . . . . ? C22 Si2 N2 Er1 -113.3(5) . . . . ? C21 Si2 N2 Er1 116.0(4) . . . . ? C19 Si1 N2 Si2 -47.0(6) . . . . ? C20 Si1 N2 Si2 74.2(6) . . . . ? C19 Si1 N2 Er1 124.0(5) . . . . ? C20 Si1 N2 Er1 -114.7(6) . . . . ? N3 Er1 N2 Si2 75.6(3) . . . . ? N1 Er1 N2 Si2 -59.8(3) . . . . ? C2 Er1 N2 Si2 -165.3(3) . . . . ? C3 Er1 N2 Si2 169.3(3) . . . . ? C4 Er1 N2 Si2 178.1(3) . . . . ? C1 Er1 N2 Si2 -136.8(3) . . . . ? C9 Er1 N2 Si2 -135.4(3) . . . . ? Si4 Er1 N2 Si2 47.3(3) . . . . ? N3 Er1 N2 Si1 -96.8(4) . . . . ? N1 Er1 N2 Si1 127.7(4) . . . . ? C2 Er1 N2 Si1 22.2(4) . . . . ? C3 Er1 N2 Si1 -3.1(5) . . . . ? C4 Er1 N2 Si1 5.7(6) . . . . ? C1 Er1 N2 Si1 50.8(5) . . . . ? C9 Er1 N2 Si1 52.2(6) . . . . ? Si2 Er1 N2 Si1 -172.5(6) . . . . ? Si4 Er1 N2 Si1 -125.1(4) . . . . ? C26 Si4 N3 Si3' -62.4(6) . . . . ? C25 Si4 N3 Si3' 69.1(6) . . . . ? Er1 Si4 N3 Si3' -166.5(6) . . . . ? C26 Si4 N3 Si3 -95.8(5) . . . . ? C25 Si4 N3 Si3 35.6(6) . . . . ? Er1 Si4 N3 Si3 160.1(6) . . . . ? C26 Si4 N3 Er1 104.1(4) . . . . ? C25 Si4 N3 Er1 -124.4(4) . . . . ? C24' Si3' N3 Si4 -150.4(8) . . . . ? C23' Si3' N3 Si4 -19.1(10) . . . . ? C24' Si3' N3 Si3 -63.4(9) . . . . ? C23' Si3' N3 Si3 68.0(9) . . . . ? C24' Si3' N3 Er1 46.1(9) . . . . ? C23' Si3' N3 Er1 177.4(8) . . . . ? C24 Si3 N3 Si4 162.2(8) . . . . ? C23 Si3 N3 Si4 59.9(8) . . . . ? C24 Si3 N3 Si3' 48.4(8) . . . . ? C23 Si3 N3 Si3' -53.9(8) . . . . ? C24 Si3 N3 Er1 -43.9(9) . . . . ? C23 Si3 N3 Er1 -146.2(7) . . . . ? N2 Er1 N3 Si4 -129.1(3) . . . . ? N1 Er1 N3 Si4 -20.9(4) . . . . ? C2 Er1 N3 Si4 133.8(3) . . . . ? C3 Er1 N3 Si4 120.5(3) . . . . ? C4 Er1 N3 Si4 90.1(3) . . . . ? C1 Er1 N3 Si4 105.4(3) . . . . ? C9 Er1 N3 Si4 75.7(3) . . . . ? Si2 Er1 N3 Si4 -96.8(2) . . . . ? N2 Er1 N3 Si3' 38.3(4) . . . . ? N1 Er1 N3 Si3' 146.5(3) . . . . ? C2 Er1 N3 Si3' -58.8(5) . . . . ? C3 Er1 N3 Si3' -72.2(4) . . . . ? C4 Er1 N3 Si3' -102.6(4) . . . . ? C1 Er1 N3 Si3' -87.2(5) . . . . ? C9 Er1 N3 Si3' -116.9(4) . . . . ? Si2 Er1 N3 Si3' 70.5(4) . . . . ? Si4 Er1 N3 Si3' 167.3(6) . . . . ? N2 Er1 N3 Si3 72.6(5) . . . . ? N1 Er1 N3 Si3 -179.2(4) . . . . ? C2 Er1 N3 Si3 -24.5(5) . . . . ? C3 Er1 N3 Si3 -37.8(5) . . . . ? C4 Er1 N3 Si3 -68.2(5) . . . . ? C1 Er1 N3 Si3 -52.9(6) . . . . ? C9 Er1 N3 Si3 -82.6(5) . . . . ? Si2 Er1 N3 Si3 104.8(4) . . . . ? Si4 Er1 N3 Si3 -158.3(6) . . . . ? N2 Er1 C1 C2 -69.2(5) . . . . ? N3 Er1 C1 C2 55.0(6) . . . . ? N1 Er1 C1 C2 -162.6(5) . . . . ? C3 Er1 C1 C2 35.6(4) . . . . ? C4 Er1 C1 C2 74.8(5) . . . . ? C9 Er1 C1 C2 112.7(7) . . . . ? Si2 Er1 C1 C2 -97.1(4) . . . . ? Si4 Er1 C1 C2 105.4(4) . . . . ? N2 Er1 C1 C9 178.1(5) . . . . ? N3 Er1 C1 C9 -57.7(6) . . . . ? N1 Er1 C1 C9 84.7(5) . . . . ? C2 Er1 C1 C9 -112.7(7) . . . . ? C3 Er1 C1 C9 -77.0(5) . . . . ? C4 Er1 C1 C9 -37.9(5) . . . . ? Si2 Er1 C1 C9 150.3(4) . . . . ? Si4 Er1 C1 C9 -7.2(6) . . . . ? N2 Er1 C1 C10 49.3(5) . . . . ? N3 Er1 C1 C10 173.6(5) . . . . ? N1 Er1 C1 C10 -44.0(5) . . . . ? C2 Er1 C1 C10 118.6(7) . . . . ? C3 Er1 C1 C10 154.2(6) . . . . ? C4 Er1 C1 C10 -166.7(6) . . . . ? C9 Er1 C1 C10 -128.8(8) . . . . ? Si2 Er1 C1 C10 21.5(6) . . . . ? Si4 Er1 C1 C10 -136.0(4) . . . . ? C9 C1 C2 C3 1.1(8) . . . . ? C10 C1 C2 C3 178.6(6) . . . . ? Er1 C1 C2 C3 -67.5(5) . . . . ? C9 C1 C2 Er1 68.5(5) . . . . ? C10 C1 C2 Er1 -114.0(6) . . . . ? N2 Er1 C2 C3 -128.4(5) . . . . ? N3 Er1 C2 C3 -26.7(5) . . . . ? N1 Er1 C2 C3 134.4(5) . . . . ? C4 Er1 C2 C3 37.7(5) . . . . ? C1 Er1 C2 C3 116.9(7) . . . . ? C9 Er1 C2 C3 79.0(5) . . . . ? Si2 Er1 C2 C3 -138.1(4) . . . . ? Si4 Er1 C2 C3 7.8(6) . . . . ? N2 Er1 C2 C1 114.7(4) . . . . ? N3 Er1 C2 C1 -143.6(4) . . . . ? N1 Er1 C2 C1 17.5(5) . . . . ? C3 Er1 C2 C1 -116.9(7) . . . . ? C4 Er1 C2 C1 -79.2(5) . . . . ? C9 Er1 C2 C1 -37.8(4) . . . . ? Si2 Er1 C2 C1 105.0(4) . . . . ? Si4 Er1 C2 C1 -109.1(4) . . . . ? C1 C2 C3 C4 -1.5(8) . . . . ? Er1 C2 C3 C4 -70.4(5) . . . . ? C1 C2 C3 Er1 68.9(5) . . . . ? N2 Er1 C3 C4 168.7(5) . . . . ? N3 Er1 C3 C4 -91.1(5) . . . . ? N1 Er1 C3 C4 55.0(5) . . . . ? C2 Er1 C3 C4 112.2(7) . . . . ? C1 Er1 C3 C4 76.7(5) . . . . ? C9 Er1 C3 C4 37.1(4) . . . . ? Si2 Er1 C3 C4 178.4(4) . . . . ? Si4 Er1 C3 C4 -62.3(5) . . . . ? N2 Er1 C3 C2 56.5(5) . . . . ? N3 Er1 C3 C2 156.7(5) . . . . ? N1 Er1 C3 C2 -57.2(5) . . . . ? C4 Er1 C3 C2 -112.2(7) . . . . ? C1 Er1 C3 C2 -35.5(4) . . . . ? C9 Er1 C3 C2 -75.1(5) . . . . ? Si2 Er1 C3 C2 66.2(5) . . . . ? Si4 Er1 C3 C2 -174.5(4) . . . . ? C2 C3 C4 C5 -178.4(8) . . . . ? Er1 C3 C4 C5 112.7(9) . . . . ? C2 C3 C4 C9 1.3(9) . . . . ? Er1 C3 C4 C9 -67.7(6) . . . . ? C2 C3 C4 Er1 68.9(5) . . . . ? N2 Er1 C4 C3 -16.5(7) . . . . ? N3 Er1 C4 C3 89.2(5) . . . . ? N1 Er1 C4 C3 -135.9(5) . . . . ? C2 Er1 C4 C3 -38.3(4) . . . . ? C1 Er1 C4 C3 -78.4(5) . . . . ? C9 Er1 C4 C3 -115.4(7) . . . . ? Si2 Er1 C4 C3 -8.1(19) . . . . ? Si4 Er1 C4 C3 121.7(5) . . . . ? N2 Er1 C4 C5 -146.5(6) . . . . ? N3 Er1 C4 C5 -40.9(7) . . . . ? N1 Er1 C4 C5 94.0(7) . . . . ? C2 Er1 C4 C5 -168.3(9) . . . . ? C3 Er1 C4 C5 -130.0(10) . . . . ? C1 Er1 C4 C5 151.6(8) . . . . ? C9 Er1 C4 C5 114.6(9) . . . . ? Si2 Er1 C4 C5 -138.1(12) . . . . ? Si4 Er1 C4 C5 -8.3(7) . . . . ? N2 Er1 C4 C9 98.9(6) . . . . ? N3 Er1 C4 C9 -155.4(5) . . . . ? N1 Er1 C4 C9 -20.5(5) . . . . ? C2 Er1 C4 C9 77.1(5) . . . . ? C3 Er1 C4 C9 115.4(7) . . . . ? C1 Er1 C4 C9 37.0(4) . . . . ? Si2 Er1 C4 C9 107.3(16) . . . . ? Si4 Er1 C4 C9 -122.9(5) . . . . ? C3 C4 C5 C6 179.5(8) . . . . ? C9 C4 C5 C6 -0.1(11) . . . . ? Er1 C4 C5 C6 -88.1(8) . . . . ? C4 C5 C6 C7 2.2(12) . . . . ? C5 C6 C7 C8 -2.6(12) . . . . ? C6 C7 C8 C9 0.9(12) . . . . ? C7 C8 C9 C1 -179.7(8) . . . . ? C7 C8 C9 C4 1.2(11) . . . . ? C7 C8 C9 Er1 86.6(8) . . . . ? C2 C1 C9 C8 -179.5(8) . . . . ? C10 C1 C9 C8 3.3(14) . . . . ? Er1 C1 C9 C8 -113.2(9) . . . . ? C2 C1 C9 C4 -0.3(8) . . . . ? C10 C1 C9 C4 -177.5(7) . . . . ? Er1 C1 C9 C4 66.1(5) . . . . ? C2 C1 C9 Er1 -66.3(5) . . . . ? C10 C1 C9 Er1 116.4(8) . . . . ? C3 C4 C9 C8 178.8(7) . . . . ? C5 C4 C9 C8 -1.5(11) . . . . ? Er1 C4 C9 C8 112.8(7) . . . . ? C3 C4 C9 C1 -0.6(9) . . . . ? C5 C4 C9 C1 179.1(7) . . . . ? Er1 C4 C9 C1 -66.6(5) . . . . ? C3 C4 C9 Er1 66.0(5) . . . . ? C5 C4 C9 Er1 -114.3(7) . . . . ? N2 Er1 C9 C8 128.6(6) . . . . ? N3 Er1 C9 C8 -86.9(6) . . . . ? N1 Er1 C9 C8 44.1(6) . . . . ? C2 Er1 C9 C8 168.9(8) . . . . ? C3 Er1 C9 C8 -151.1(7) . . . . ? C4 Er1 C9 C8 -115.3(8) . . . . ? C1 Er1 C9 C8 131.2(9) . . . . ? Si2 Er1 C9 C8 78.1(7) . . . . ? Si4 Er1 C9 C8 -53.9(6) . . . . ? N2 Er1 C9 C1 -2.6(6) . . . . ? N3 Er1 C9 C1 141.9(4) . . . . ? N1 Er1 C9 C1 -87.0(5) . . . . ? C2 Er1 C9 C1 37.7(4) . . . . ? C3 Er1 C9 C1 77.8(5) . . . . ? C4 Er1 C9 C1 113.5(7) . . . . ? Si2 Er1 C9 C1 -53.1(7) . . . . ? Si4 Er1 C9 C1 174.9(4) . . . . ? N2 Er1 C9 C4 -116.1(5) . . . . ? N3 Er1 C9 C4 28.4(5) . . . . ? N1 Er1 C9 C4 159.5(5) . . . . ? C2 Er1 C9 C4 -75.7(5) . . . . ? C3 Er1 C9 C4 -35.7(4) . . . . ? C1 Er1 C9 C4 -113.5(7) . . . . ? Si2 Er1 C9 C4 -166.6(4) . . . . ? Si4 Er1 C9 C4 61.4(5) . . . . ? C2 C1 C10 C18 -140.8(7) . . . . ? C9 C1 C10 C18 36.0(11) . . . . ? Er1 C1 C10 C18 132.0(6) . . . . ? C2 C1 C10 C11 96.2(8) . . . . ? C9 C1 C10 C11 -87.0(10) . . . . ? Er1 C1 C10 C11 9.0(8) . . . . ? C2 C1 C10 C17 -20.7(10) . . . . ? C9 C1 C10 C17 156.1(8) . . . . ? Er1 C1 C10 C17 -107.9(6) . . . . ? C1 C10 C11 C12 63.7(9) . . . . ? C18 C10 C11 C12 -59.8(9) . . . . ? C17 C10 C11 C12 -177.1(7) . . . . ? C16 N1 C12 C13 2.2(10) . . . . ? Er1 N1 C12 C13 -171.8(6) . . . . ? C16 N1 C12 C11 -176.6(6) . . . . ? Er1 N1 C12 C11 9.4(8) . . . . ? C10 C11 C12 C13 100.6(9) . . . . ? C10 C11 C12 N1 -80.6(8) . . . . ? N1 C12 C13 C14 0.6(13) . . . . ? C11 C12 C13 C14 179.4(8) . . . . ? C12 C13 C14 C15 -2.5(14) . . . . ? C13 C14 C15 C16 1.4(13) . . . . ? C12 N1 C16 C15 -3.4(10) . . . . ? Er1 N1 C16 C15 170.8(6) . . . . ? C14 C15 C16 N1 1.6(12) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.374 _refine_diff_density_min -1.424 _refine_diff_density_rms 0.105 data_shelxl4 _database_code_depnum_ccdc_archive 'CCDC 900283' #TrackingRef 'CCDC 900280.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H46 Lu N3 Si4' _chemical_formula_sum 'C26 H46 Lu N3 Si4' _chemical_formula_weight 687.99 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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' '-x, -y, z+1/2' _cell_length_a 16.314(5) _cell_length_b 10.921(4) _cell_length_c 18.668(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3325.8(18) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9673 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 3.130 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.141 _exptl_absorpt_correction_T_max 0.391 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9575 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.49 _reflns_number_total 5270 _reflns_number_gt 4395 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.064(17) _refine_ls_number_reflns 5270 _refine_ls_number_parameters 250 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1111 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Lu1 Lu 0.16580(2) 0.45737(3) 0.31417(5) 0.03962(13) Uani 1 1 d . A . Si1 Si 0.1449(2) 0.3171(4) 0.48591(18) 0.0676(9) Uani 1 1 d D . . H1 H 0.073(4) 0.399(8) 0.494(3) 0.081 Uiso 1 1 d D . . Si2 Si 0.3045(2) 0.3675(3) 0.41205(17) 0.0556(8) Uani 1 1 d D . . H2 H 0.327(6) 0.423(8) 0.343(3) 0.067 Uiso 1 1 d D . . Si3 Si 0.1740(3) 0.1598(4) 0.2421(3) 0.1021(16) Uani 1 1 d D . . H3 H 0.185(7) 0.110(11) 0.315(3) 0.122 Uiso 1 1 d D . . Si4 Si 0.2326(2) 0.3867(5) 0.1649(2) 0.0823(12) Uani 1 1 d D . . H4 H 0.227(8) 0.516(4) 0.188(6) 0.099 Uiso 1 1 d D . . N1 N 0.2454(4) 0.6422(7) 0.3284(5) 0.046(2) Uani 1 1 d . . . N2 N 0.2010(6) 0.3761(8) 0.4175(5) 0.050(2) Uani 1 1 d . A . N3 N 0.1942(7) 0.3158(11) 0.2358(5) 0.067(3) Uani 1 1 d . A . C1 C 0.0547(9) 0.6246(13) 0.3509(8) 0.0554(9) Uani 1 1 d . . . C2 C 0.0211(7) 0.5019(12) 0.3648(7) 0.0554(9) Uani 1 1 d . A . H2A H 0.0011 0.4734 0.4120 0.066 Uiso 1 1 calc R . . C3 C 0.0084(6) 0.4407(9) 0.3004(6) 0.0554(9) Uani 1 1 d . . . H3A H -0.0230 0.3638 0.2944 0.066 Uiso 1 1 calc R A . C4 C 0.0300(8) 0.5229(11) 0.2451(7) 0.0554(9) Uani 1 1 d . A . C5 C 0.0261(7) 0.5119(11) 0.1674(6) 0.0554(9) Uani 1 1 d . . . H5 H 0.0081 0.4390 0.1457 0.066 Uiso 1 1 calc R A . C6 C 0.0489(7) 0.6082(10) 0.1278(6) 0.0554(9) Uani 1 1 d . A . H6 H 0.0451 0.6025 0.0776 0.066 Uiso 1 1 calc R . . C7 C 0.0777(7) 0.7154(10) 0.1575(7) 0.0554(9) Uani 1 1 d . . . H7 H 0.0929 0.7809 0.1276 0.066 Uiso 1 1 calc R A . C8 C 0.0840(8) 0.7268(13) 0.2284(8) 0.0554(9) Uani 1 1 d . A . H8 H 0.1063 0.7990 0.2477 0.066 Uiso 1 1 calc R . . C9 C 0.0581(9) 0.6338(13) 0.2748(7) 0.0554(9) Uani 1 1 d . A . C10 C 0.0753(8) 0.7145(11) 0.4104(7) 0.057(3) Uani 1 1 d . A . C11 C 0.1666(7) 0.7049(10) 0.4340(5) 0.053(3) Uani 1 1 d . . . H11A H 0.1759 0.7619 0.4737 0.064 Uiso 1 1 calc R A . H11B H 0.1766 0.6219 0.4520 0.064 Uiso 1 1 calc R . . C12 C 0.2270(7) 0.7315(11) 0.3770(6) 0.0633(14) Uani 1 1 d . A . C13 C 0.2694(7) 0.8382(11) 0.3777(6) 0.0633(14) Uani 1 1 d . . . H13 H 0.2559 0.8976 0.4122 0.076 Uiso 1 1 calc R A . C14 C 0.3317(6) 0.8629(12) 0.3297(6) 0.0633(14) Uani 1 1 d . A . H14 H 0.3606 0.9374 0.3312 0.076 Uiso 1 1 calc R . . C15 C 0.3497(8) 0.7762(12) 0.2805(6) 0.0633(14) Uani 1 1 d . . . H15 H 0.3912 0.7899 0.2464 0.076 Uiso 1 1 calc R A . C16 C 0.3049(8) 0.6630(12) 0.2805(6) 0.0633(14) Uani 1 1 d . A . H16 H 0.3176 0.6025 0.2464 0.076 Uiso 1 1 calc R . . C17 C 0.0245(8) 0.6867(12) 0.4776(6) 0.068(3) Uani 1 1 d . . . H17A H -0.0323 0.7090 0.4692 0.101 Uiso 1 1 calc R A . H17B H 0.0456 0.7337 0.5177 0.101 Uiso 1 1 calc R . . H17C H 0.0279 0.6001 0.4885 0.101 Uiso 1 1 calc R . . C18 C 0.0572(9) 0.8470(10) 0.3863(8) 0.088(4) Uani 1 1 d . . . H18A H 0.0029 0.8508 0.3652 0.132 Uiso 1 1 calc R A . H18B H 0.0976 0.8722 0.3512 0.132 Uiso 1 1 calc R . . H18C H 0.0597 0.9012 0.4274 0.132 Uiso 1 1 calc R . . C19 C 0.0705(19) 0.199(3) 0.4597(19) 0.100(7) Uiso 0.50 1 d PD A 1 H19A H 0.0993 0.1238 0.4479 0.149 Uiso 0.50 1 calc PR A 1 H19B H 0.0397 0.2266 0.4184 0.149 Uiso 0.50 1 calc PR A 1 H19C H 0.0332 0.1836 0.4992 0.149 Uiso 0.50 1 calc PR A 1 C19' C 0.110(2) 0.1548(19) 0.4721(18) 0.100(7) Uiso 0.50 1 d PD A 2 H19D H 0.0937 0.1435 0.4226 0.149 Uiso 0.50 1 calc PR A 2 H19E H 0.0637 0.1379 0.5032 0.149 Uiso 0.50 1 calc PR A 2 H19F H 0.1545 0.0992 0.4835 0.149 Uiso 0.50 1 calc PR A 2 C20 C 0.2052(19) 0.261(3) 0.5630(13) 0.087(7) Uiso 0.50 1 d PD A 1 H20A H 0.2346 0.1873 0.5494 0.131 Uiso 0.50 1 calc PR A 1 H20B H 0.1685 0.2426 0.6025 0.131 Uiso 0.50 1 calc PR A 1 H20C H 0.2440 0.3233 0.5776 0.131 Uiso 0.50 1 calc PR A 1 C20' C 0.1935(19) 0.322(3) 0.5730(11) 0.087(7) Uiso 0.50 1 d PD A 2 H20D H 0.2380 0.2637 0.5746 0.131 Uiso 0.50 1 calc PR A 2 H20E H 0.1536 0.3026 0.6097 0.131 Uiso 0.50 1 calc PR A 2 H20F H 0.2149 0.4041 0.5814 0.131 Uiso 0.50 1 calc PR A 2 C21 C 0.3613(9) 0.4697(13) 0.4756(9) 0.081(4) Uani 1 1 d . A . H21A H 0.3436 0.5537 0.4688 0.121 Uiso 1 1 calc R . . H21B H 0.4197 0.4638 0.4663 0.121 Uiso 1 1 calc R . . H21C H 0.3501 0.4446 0.5244 0.121 Uiso 1 1 calc R . . C22 C 0.3509(10) 0.2097(14) 0.4191(8) 0.102(5) Uani 1 1 d . A . H22A H 0.3140 0.1566 0.4455 0.153 Uiso 1 1 calc R . . H22B H 0.4029 0.2147 0.4440 0.153 Uiso 1 1 calc R . . H22C H 0.3595 0.1767 0.3715 0.153 Uiso 1 1 calc R . . C23 C 0.263(2) 0.078(5) 0.199(3) 0.142(11) Uiso 0.50 1 d PD B 1 H23A H 0.3128 0.1227 0.2072 0.213 Uiso 0.50 1 calc PR B 1 H23B H 0.2531 0.0717 0.1473 0.213 Uiso 0.50 1 calc PR B 1 H23C H 0.2674 -0.0041 0.2186 0.213 Uiso 0.50 1 calc PR B 1 C23' C 0.236(3) 0.052(4) 0.187(3) 0.142(11) Uiso 0.50 1 d PD B 2 H23D H 0.2106 0.0431 0.1403 0.213 Uiso 0.50 1 calc PR B 2 H23E H 0.2383 -0.0267 0.2107 0.213 Uiso 0.50 1 calc PR B 2 H23F H 0.2909 0.0846 0.1814 0.213 Uiso 0.50 1 calc PR B 2 C24 C 0.0831(19) 0.120(4) 0.188(2) 0.129(11) Uiso 0.50 1 d PD B 1 H24A H 0.0355 0.1156 0.2194 0.194 Uiso 0.50 1 calc PR B 1 H24B H 0.0916 0.0418 0.1653 0.194 Uiso 0.50 1 calc PR B 1 H24C H 0.0743 0.1828 0.1523 0.194 Uiso 0.50 1 calc PR B 1 C24' C 0.0640(14) 0.111(4) 0.240(2) 0.129(11) Uiso 0.50 1 d PD B 2 H24D H 0.0343 0.1621 0.2058 0.194 Uiso 0.50 1 calc PR B 2 H24E H 0.0402 0.1202 0.2869 0.194 Uiso 0.50 1 calc PR B 2 H24F H 0.0606 0.0263 0.2248 0.194 Uiso 0.50 1 calc PR B 2 C25 C 0.187(3) 0.384(3) 0.0738(13) 0.081(6) Uiso 0.50 1 d PD A 1 H25A H 0.1774 0.2995 0.0594 0.122 Uiso 0.50 1 calc PR A 1 H25B H 0.2241 0.4224 0.0402 0.122 Uiso 0.50 1 calc PR A 1 H25C H 0.1352 0.4277 0.0742 0.122 Uiso 0.50 1 calc PR A 1 C25' C 0.178(3) 0.346(3) 0.0792(15) 0.081(6) Uiso 0.50 1 d PD A 2 H25D H 0.2063 0.2782 0.0560 0.122 Uiso 0.50 1 calc PR A 2 H25E H 0.1776 0.4160 0.0474 0.122 Uiso 0.50 1 calc PR A 2 H25F H 0.1221 0.3216 0.0899 0.122 Uiso 0.50 1 calc PR A 2 C26 C 0.3466(12) 0.399(4) 0.152(2) 0.095(8) Uiso 0.50 1 d PD A 1 H26A H 0.3733 0.3968 0.1988 0.143 Uiso 0.50 1 calc PR A 1 H26B H 0.3595 0.4749 0.1283 0.143 Uiso 0.50 1 calc PR A 1 H26C H 0.3657 0.3303 0.1237 0.143 Uiso 0.50 1 calc PR A 1 C26' C 0.3421(12) 0.339(3) 0.154(2) 0.095(8) Uiso 0.50 1 d PD A 2 H26D H 0.3761 0.3873 0.1866 0.143 Uiso 0.50 1 calc PR A 2 H26E H 0.3594 0.3532 0.1054 0.143 Uiso 0.50 1 calc PR A 2 H26F H 0.3476 0.2532 0.1660 0.143 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.03542(19) 0.0435(2) 0.0400(2) -0.0022(3) 0.0039(3) 0.00277(15) Si1 0.071(2) 0.083(2) 0.0489(19) 0.0160(18) 0.0072(16) 0.0039(19) Si2 0.0537(18) 0.0575(18) 0.0556(19) -0.0012(16) 0.0008(15) 0.0105(16) Si3 0.146(5) 0.080(3) 0.080(3) -0.034(2) -0.021(3) 0.015(3) Si4 0.059(2) 0.125(4) 0.062(2) -0.033(2) -0.0004(18) 0.013(2) N1 0.024(3) 0.060(5) 0.055(7) 0.006(5) 0.005(4) -0.013(3) N2 0.054(6) 0.055(6) 0.040(5) -0.005(4) -0.007(4) 0.008(5) N3 0.068(7) 0.093(8) 0.039(5) -0.015(6) -0.008(5) 0.000(6) C1 0.0453(18) 0.057(2) 0.064(2) 0.000(2) -0.002(2) 0.0031(17) C2 0.0453(18) 0.057(2) 0.064(2) 0.000(2) -0.002(2) 0.0031(17) C3 0.0453(18) 0.057(2) 0.064(2) 0.000(2) -0.002(2) 0.0031(17) C4 0.0453(18) 0.057(2) 0.064(2) 0.000(2) -0.002(2) 0.0031(17) C5 0.0453(18) 0.057(2) 0.064(2) 0.000(2) -0.002(2) 0.0031(17) C6 0.0453(18) 0.057(2) 0.064(2) 0.000(2) -0.002(2) 0.0031(17) C7 0.0453(18) 0.057(2) 0.064(2) 0.000(2) -0.002(2) 0.0031(17) C8 0.0453(18) 0.057(2) 0.064(2) 0.000(2) -0.002(2) 0.0031(17) C9 0.0453(18) 0.057(2) 0.064(2) 0.000(2) -0.002(2) 0.0031(17) C10 0.063(8) 0.041(6) 0.065(8) -0.015(6) 0.012(6) 0.001(5) C11 0.062(7) 0.052(6) 0.046(6) -0.007(5) -0.009(5) -0.016(5) C12 0.056(3) 0.072(4) 0.062(3) 0.012(3) -0.005(3) -0.013(3) C13 0.056(3) 0.072(4) 0.062(3) 0.012(3) -0.005(3) -0.013(3) C14 0.056(3) 0.072(4) 0.062(3) 0.012(3) -0.005(3) -0.013(3) C15 0.056(3) 0.072(4) 0.062(3) 0.012(3) -0.005(3) -0.013(3) C16 0.056(3) 0.072(4) 0.062(3) 0.012(3) -0.005(3) -0.013(3) C17 0.068(8) 0.073(8) 0.062(7) -0.021(6) 0.029(6) -0.005(7) C18 0.085(10) 0.049(7) 0.129(13) -0.035(8) -0.020(9) 0.004(7) C21 0.048(8) 0.086(10) 0.108(13) -0.022(9) -0.026(8) 0.007(7) C22 0.113(13) 0.077(10) 0.117(13) -0.002(9) -0.009(10) 0.045(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 N3 2.179(10) . ? Lu1 N2 2.199(9) . ? Lu1 N1 2.415(7) . ? Lu1 C3 2.587(10) . ? Lu1 C2 2.588(13) . ? Lu1 C4 2.661(13) . ? Lu1 C1 2.663(14) . ? Lu1 C9 2.709(14) . ? Lu1 Si2 3.070(3) . ? Lu1 Si4 3.090(4) . ? Si1 N2 1.698(10) . ? Si1 C20' 1.809(17) . ? Si1 C19 1.839(18) . ? Si1 C20 1.848(17) . ? Si1 C19' 1.880(18) . ? Si1 H1 1.483(10) . ? Si2 N2 1.694(10) . ? Si2 C21 1.874(13) . ? Si2 C22 1.886(14) . ? Si2 H2 1.481(10) . ? Si3 N3 1.739(12) . ? Si3 C24 1.840(18) . ? Si3 C23' 1.857(19) . ? Si3 C24' 1.870(18) . ? Si3 C23 1.886(19) . ? Si3 H3 1.481(10) . ? Si4 N3 1.656(12) . ? Si4 C25 1.857(17) . ? Si4 C26' 1.869(17) . ? Si4 C26 1.878(18) . ? Si4 C25' 1.886(17) . ? Si4 H4 1.481(10) . ? N1 C16 1.339(14) . ? N1 C12 1.365(15) . ? C1 C9 1.425(12) . ? C1 C2 1.470(19) . ? C1 C10 1.520(18) . ? C2 C3 1.391(16) . ? C2 H2A 0.9900 . ? C3 C4 1.414(15) . ? C3 H3A 0.9900 . ? C4 C9 1.409(19) . ? C4 C5 1.456(17) . ? C5 C6 1.339(15) . ? C5 H5 0.9400 . ? C6 C7 1.378(16) . ? C6 H6 0.9400 . ? C7 C8 1.334(18) . ? C7 H7 0.9400 . ? C8 C9 1.400(19) . ? C8 H8 0.9400 . ? C10 C17 1.534(16) . ? C10 C18 1.543(17) . ? C10 C11 1.558(16) . ? C11 C12 1.479(15) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.356(16) . ? C13 C14 1.383(15) . ? C13 H13 0.9400 . ? C14 C15 1.351(16) . ? C14 H14 0.9400 . ? C15 C16 1.436(17) . ? C15 H15 0.9400 . ? C16 H16 0.9400 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C19' H19D 0.9700 . ? C19' H19E 0.9700 . ? C19' H19F 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C20' H20D 0.9700 . ? C20' H20E 0.9700 . ? C20' H20F 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C23' H23D 0.9700 . ? C23' H23E 0.9700 . ? C23' H23F 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C24' H24D 0.9700 . ? C24' H24E 0.9700 . ? C24' H24F 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C25' H25D 0.9700 . ? C25' H25E 0.9700 . ? C25' H25F 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C26' H26D 0.9700 . ? C26' H26E 0.9700 . ? C26' H26F 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Lu1 N2 104.3(4) . . ? N3 Lu1 N1 123.6(4) . . ? N2 Lu1 N1 95.8(3) . . ? N3 Lu1 C3 95.4(4) . . ? N2 Lu1 C3 108.5(4) . . ? N1 Lu1 C3 127.1(3) . . ? N3 Lu1 C2 124.9(4) . . ? N2 Lu1 C2 89.6(4) . . ? N1 Lu1 C2 107.0(3) . . ? C3 Lu1 C2 31.2(4) . . ? N3 Lu1 C4 92.4(4) . . ? N2 Lu1 C4 138.7(4) . . ? N1 Lu1 C4 106.0(3) . . ? C3 Lu1 C4 31.2(3) . . ? C2 Lu1 C4 50.8(3) . . ? N3 Lu1 C1 143.5(4) . . ? N2 Lu1 C1 103.2(4) . . ? N1 Lu1 C1 76.4(4) . . ? C3 Lu1 C1 53.0(4) . . ? C2 Lu1 C1 32.5(4) . . ? C4 Lu1 C1 51.2(4) . . ? N3 Lu1 C9 117.4(4) . . ? N2 Lu1 C9 134.0(4) . . ? N1 Lu1 C9 77.5(4) . . ? C3 Lu1 C9 51.6(4) . . ? C2 Lu1 C9 51.2(4) . . ? C4 Lu1 C9 30.4(4) . . ? C1 Lu1 C9 30.7(3) . . ? N3 Lu1 Si2 90.9(3) . . ? N2 Lu1 Si2 32.5(3) . . ? N1 Lu1 Si2 78.8(2) . . ? C3 Lu1 Si2 140.2(2) . . ? C2 Lu1 Si2 121.0(3) . . ? C4 Lu1 Si2 171.1(3) . . ? C1 Lu1 Si2 124.6(3) . . ? C9 Lu1 Si2 150.1(3) . . ? N3 Lu1 Si4 30.9(3) . . ? N2 Lu1 Si4 126.7(2) . . ? N1 Lu1 Si4 96.8(2) . . ? C3 Lu1 Si4 104.1(3) . . ? C2 Lu1 Si4 134.3(3) . . ? C4 Lu1 Si4 85.6(3) . . ? C1 Lu1 Si4 130.1(3) . . ? C9 Lu1 Si4 99.3(3) . . ? Si2 Lu1 Si4 101.35(10) . . ? N2 Si1 C20' 115.3(12) . . ? N2 Si1 C19 115.0(12) . . ? C20' Si1 C19 123.4(17) . . ? N2 Si1 C20 115.2(12) . . ? C20' Si1 C20 22.8(14) . . ? C19 Si1 C20 109.0(16) . . ? N2 Si1 C19' 114.7(11) . . ? C20' Si1 C19' 106.6(16) . . ? C19 Si1 C19' 26.0(14) . . ? C20 Si1 C19' 87.4(16) . . ? N2 Si1 H1 106(4) . . ? C20' Si1 H1 103.7(11) . . ? C19 Si1 H1 86(4) . . ? C20 Si1 H1 123(2) . . ? C19' Si1 H1 110(4) . . ? N2 Si2 C21 115.0(6) . . ? N2 Si2 C22 116.5(7) . . ? C21 Si2 C22 107.6(7) . . ? N2 Si2 Lu1 44.2(3) . . ? C21 Si2 Lu1 123.4(4) . . ? C22 Si2 Lu1 129.0(5) . . ? N2 Si2 H2 106(4) . . ? C21 Si2 H2 101(4) . . ? C22 Si2 H2 110(4) . . ? Lu1 Si2 H2 62(4) . . ? N3 Si3 C24 110.2(15) . . ? N3 Si3 C23' 118.6(18) . . ? C24 Si3 C23' 89(2) . . ? N3 Si3 C24' 117.2(15) . . ? C24 Si3 C24' 31.6(14) . . ? C23' Si3 C24' 109(2) . . ? N3 Si3 C23 107.0(18) . . ? C24 Si3 C23 106(2) . . ? C23' Si3 C23 17(3) . . ? C24' Si3 C23 126(2) . . ? N3 Si3 H3 113(5) . . ? C24 Si3 H3 121(5) . . ? C23' Si3 H3 102(5) . . ? C24' Si3 H3 92(5) . . ? C23 Si3 H3 98(5) . . ? N3 Si4 C25 124.8(13) . . ? N3 Si4 C26' 108.4(13) . . ? C25 Si4 C26' 106.5(19) . . ? N3 Si4 C26 120.4(14) . . ? C25 Si4 C26 107(2) . . ? C26' Si4 C26 20.0(16) . . ? N3 Si4 C25' 112.8(14) . . ? C25 Si4 C25' 13.8(19) . . ? C26' Si4 C25' 107.3(19) . . ? C26 Si4 C25' 112.3(19) . . ? N3 Si4 Lu1 42.5(4) . . ? C25 Si4 Lu1 133.5(15) . . ? C26' Si4 Lu1 120.0(12) . . ? C26 Si4 Lu1 116.3(13) . . ? C25' Si4 Lu1 131.2(15) . . ? N3 Si4 H4 101(5) . . ? C25 Si4 H4 105(5) . . ? C26' Si4 H4 111(5) . . ? C26 Si4 H4 92(5) . . ? C25' Si4 H4 116(5) . . ? Lu1 Si4 H4 59(5) . . ? C16 N1 C12 118.8(9) . . ? C16 N1 Lu1 117.3(8) . . ? C12 N1 Lu1 123.5(6) . . ? Si2 N2 Si1 124.1(6) . . ? Si2 N2 Lu1 103.3(5) . . ? Si1 N2 Lu1 132.2(6) . . ? Si4 N3 Si3 125.7(6) . . ? Si4 N3 Lu1 106.6(6) . . ? Si3 N3 Lu1 127.6(6) . . ? C9 C1 C2 104.8(13) . . ? C9 C1 C10 132.4(15) . . ? C2 C1 C10 122.8(12) . . ? C9 C1 Lu1 76.4(10) . . ? C2 C1 Lu1 71.0(7) . . ? C10 C1 Lu1 118.7(9) . . ? C3 C2 C1 110.0(11) . . ? C3 C2 Lu1 74.4(7) . . ? C1 C2 Lu1 76.5(8) . . ? C3 C2 H2A 124.6 . . ? C1 C2 H2A 124.6 . . ? Lu1 C2 H2A 124.6 . . ? C2 C3 C4 106.8(9) . . ? C2 C3 Lu1 74.5(7) . . ? C4 C3 Lu1 77.3(7) . . ? C2 C3 H3A 125.7 . . ? C4 C3 H3A 125.7 . . ? Lu1 C3 H3A 125.7 . . ? C9 C4 C3 109.8(11) . . ? C9 C4 C5 118.6(11) . . ? C3 C4 C5 131.6(11) . . ? C9 C4 Lu1 76.7(8) . . ? C3 C4 Lu1 71.5(6) . . ? C5 C4 Lu1 119.8(8) . . ? C6 C5 C4 118.2(11) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? C5 C6 C7 122.7(11) . . ? C5 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C8 C7 C6 120.3(12) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 121.5(14) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C8 C9 C4 118.6(13) . . ? C8 C9 C1 132.8(16) . . ? C4 C9 C1 108.6(14) . . ? C8 C9 Lu1 119.2(10) . . ? C4 C9 Lu1 72.9(7) . . ? C1 C9 Lu1 72.8(10) . . ? C1 C10 C17 110.5(11) . . ? C1 C10 C18 110.5(11) . . ? C17 C10 C18 108.7(11) . . ? C1 C10 C11 112.0(10) . . ? C17 C10 C11 105.8(11) . . ? C18 C10 C11 109.2(11) . . ? C12 C11 C10 114.8(9) . . ? C12 C11 H11A 108.6 . . ? C10 C11 H11A 108.6 . . ? C12 C11 H11B 108.6 . . ? C10 C11 H11B 108.6 . . ? H11A C11 H11B 107.5 . . ? C13 C12 N1 120.6(11) . . ? C13 C12 C11 120.1(12) . . ? N1 C12 C11 119.0(10) . . ? C12 C13 C14 122.4(13) . . ? C12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C15 C14 C13 117.6(11) . . ? C15 C14 H14 121.2 . . ? C13 C14 H14 121.2 . . ? C14 C15 C16 119.5(12) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? N1 C16 C15 121.0(12) . . ? N1 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 C18 H18A 109.5 . . ? C10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C10 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? Si1 C19 H19C 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 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? Si1 C20 H20C 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 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 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C23' H23D 109.5 . . ? Si3 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? Si3 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? Si3 C24 H24A 109.5 . . ? Si3 C24 H24B 109.5 . . ? Si3 C24 H24C 109.5 . . ? Si3 C24' H24D 109.5 . . ? Si3 C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? Si3 C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? Si4 C25 H25A 109.5 . . ? Si4 C25 H25B 109.5 . . ? Si4 C25 H25C 109.5 . . ? Si4 C25' H25D 109.5 . . ? Si4 C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? Si4 C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? Si4 C26' H26D 109.5 . . ? Si4 C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? Si4 C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 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 Lu1 Si2 N2 -115.8(6) . . . . ? N1 Lu1 Si2 N2 120.2(5) . . . . ? C3 Lu1 Si2 N2 -16.2(6) . . . . ? C2 Lu1 Si2 N2 16.9(5) . . . . ? C4 Lu1 Si2 N2 -4(2) . . . . ? C1 Lu1 Si2 N2 55.5(6) . . . . ? C9 Lu1 Si2 N2 82.0(8) . . . . ? Si4 Lu1 Si2 N2 -145.1(4) . . . . ? N3 Lu1 Si2 C21 151.5(7) . . . . ? N2 Lu1 Si2 C21 -92.7(8) . . . . ? N1 Lu1 Si2 C21 27.4(7) . . . . ? C3 Lu1 Si2 C21 -108.9(8) . . . . ? C2 Lu1 Si2 C21 -75.8(8) . . . . ? C4 Lu1 Si2 C21 -96(2) . . . . ? C1 Lu1 Si2 C21 -37.2(8) . . . . ? C9 Lu1 Si2 C21 -10.7(9) . . . . ? Si4 Lu1 Si2 C21 122.2(7) . . . . ? N3 Lu1 Si2 C22 -26.3(8) . . . . ? N2 Lu1 Si2 C22 89.5(8) . . . . ? N1 Lu1 Si2 C22 -150.4(7) . . . . ? C3 Lu1 Si2 C22 73.3(8) . . . . ? C2 Lu1 Si2 C22 106.4(8) . . . . ? C4 Lu1 Si2 C22 86(2) . . . . ? C1 Lu1 Si2 C22 145.0(8) . . . . ? C9 Lu1 Si2 C22 171.5(9) . . . . ? Si4 Lu1 Si2 C22 -55.6(7) . . . . ? N2 Lu1 Si4 N3 49.8(7) . . . . ? N1 Lu1 Si4 N3 152.2(6) . . . . ? C3 Lu1 Si4 N3 -76.7(6) . . . . ? C2 Lu1 Si4 N3 -85.9(7) . . . . ? C4 Lu1 Si4 N3 -102.1(6) . . . . ? C1 Lu1 Si4 N3 -129.9(7) . . . . ? C9 Lu1 Si4 N3 -129.3(7) . . . . ? Si2 Lu1 Si4 N3 72.4(6) . . . . ? N3 Lu1 Si4 C25 97.5(16) . . . . ? N2 Lu1 Si4 C25 147.3(15) . . . . ? N1 Lu1 Si4 C25 -110.3(15) . . . . ? C3 Lu1 Si4 C25 20.8(15) . . . . ? C2 Lu1 Si4 C25 11.6(16) . . . . ? C4 Lu1 Si4 C25 -4.6(15) . . . . ? C1 Lu1 Si4 C25 -32.4(16) . . . . ? C9 Lu1 Si4 C25 -31.9(15) . . . . ? Si2 Lu1 Si4 C25 169.8(15) . . . . ? N3 Lu1 Si4 C26' -84.9(14) . . . . ? N2 Lu1 Si4 C26' -35.0(14) . . . . ? N1 Lu1 Si4 C26' 67.4(13) . . . . ? C3 Lu1 Si4 C26' -161.6(13) . . . . ? C2 Lu1 Si4 C26' -170.7(13) . . . . ? C4 Lu1 Si4 C26' 173.0(13) . . . . ? C1 Lu1 Si4 C26' 145.3(13) . . . . ? C9 Lu1 Si4 C26' 145.8(13) . . . . ? Si2 Lu1 Si4 C26' -12.5(13) . . . . ? N3 Lu1 Si4 C26 -107.2(15) . . . . ? N2 Lu1 Si4 C26 -57.4(15) . . . . ? N1 Lu1 Si4 C26 45.0(14) . . . . ? C3 Lu1 Si4 C26 176.0(14) . . . . ? C2 Lu1 Si4 C26 166.9(15) . . . . ? C4 Lu1 Si4 C26 150.6(14) . . . . ? C1 Lu1 Si4 C26 122.9(15) . . . . ? C9 Lu1 Si4 C26 123.4(15) . . . . ? Si2 Lu1 Si4 C26 -34.9(14) . . . . ? N3 Lu1 Si4 C25' 79.0(17) . . . . ? N2 Lu1 Si4 C25' 128.8(16) . . . . ? N1 Lu1 Si4 C25' -128.8(16) . . . . ? C3 Lu1 Si4 C25' 2.3(16) . . . . ? C2 Lu1 Si4 C25' -6.9(17) . . . . ? C4 Lu1 Si4 C25' -23.1(16) . . . . ? C1 Lu1 Si4 C25' -50.9(16) . . . . ? C9 Lu1 Si4 C25' -50.3(16) . . . . ? Si2 Lu1 Si4 C25' 151.4(16) . . . . ? N3 Lu1 N1 C16 6.8(9) . . . . ? N2 Lu1 N1 C16 118.2(8) . . . . ? C3 Lu1 N1 C16 -123.3(8) . . . . ? C2 Lu1 N1 C16 -150.4(8) . . . . ? C4 Lu1 N1 C16 -97.3(8) . . . . ? C1 Lu1 N1 C16 -139.5(9) . . . . ? C9 Lu1 N1 C16 -108.0(9) . . . . ? Si2 Lu1 N1 C16 90.4(8) . . . . ? Si4 Lu1 N1 C16 -9.9(8) . . . . ? N3 Lu1 N1 C12 179.2(8) . . . . ? N2 Lu1 N1 C12 -69.4(9) . . . . ? C3 Lu1 N1 C12 49.1(10) . . . . ? C2 Lu1 N1 C12 22.0(9) . . . . ? C4 Lu1 N1 C12 75.1(9) . . . . ? C1 Lu1 N1 C12 32.8(8) . . . . ? C9 Lu1 N1 C12 64.4(8) . . . . ? Si2 Lu1 N1 C12 -97.2(8) . . . . ? Si4 Lu1 N1 C12 162.5(8) . . . . ? C21 Si2 N2 Si1 -73.0(9) . . . . ? C22 Si2 N2 Si1 54.2(9) . . . . ? Lu1 Si2 N2 Si1 173.9(9) . . . . ? C21 Si2 N2 Lu1 113.1(7) . . . . ? C22 Si2 N2 Lu1 -119.7(6) . . . . ? C20' Si1 N2 Si2 34.0(14) . . . . ? C19 Si1 N2 Si2 -119.2(14) . . . . ? C20 Si1 N2 Si2 8.7(14) . . . . ? C19' Si1 N2 Si2 -90.6(14) . . . . ? C20' Si1 N2 Lu1 -154.0(13) . . . . ? C19 Si1 N2 Lu1 52.8(15) . . . . ? C20 Si1 N2 Lu1 -179.2(13) . . . . ? C19' Si1 N2 Lu1 81.5(14) . . . . ? N3 Lu1 N2 Si2 68.3(5) . . . . ? N1 Lu1 N2 Si2 -58.5(4) . . . . ? C3 Lu1 N2 Si2 169.2(4) . . . . ? C2 Lu1 N2 Si2 -165.6(5) . . . . ? C4 Lu1 N2 Si2 179.2(5) . . . . ? C1 Lu1 N2 Si2 -135.8(5) . . . . ? C9 Lu1 N2 Si2 -136.7(5) . . . . ? Si4 Lu1 N2 Si2 44.4(5) . . . . ? N3 Lu1 N2 Si1 -104.9(6) . . . . ? N1 Lu1 N2 Si1 128.3(6) . . . . ? C3 Lu1 N2 Si1 -4.1(7) . . . . ? C2 Lu1 N2 Si1 21.2(7) . . . . ? C4 Lu1 N2 Si1 5.9(10) . . . . ? C1 Lu1 N2 Si1 51.0(7) . . . . ? C9 Lu1 N2 Si1 50.0(9) . . . . ? Si2 Lu1 N2 Si1 -173.2(10) . . . . ? Si4 Lu1 N2 Si1 -128.8(5) . . . . ? C25 Si4 N3 Si3 56.9(19) . . . . ? C26' Si4 N3 Si3 -69.7(14) . . . . ? C26 Si4 N3 Si3 -87.4(17) . . . . ? C25' Si4 N3 Si3 49.0(17) . . . . ? Lu1 Si4 N3 Si3 175.7(12) . . . . ? C25 Si4 N3 Lu1 -118.8(17) . . . . ? C26' Si4 N3 Lu1 114.6(13) . . . . ? C26 Si4 N3 Lu1 96.9(16) . . . . ? C25' Si4 N3 Lu1 -126.7(15) . . . . ? C24 Si3 N3 Si4 -73.1(17) . . . . ? C23' Si3 N3 Si4 28(2) . . . . ? C24' Si3 N3 Si4 -106.8(16) . . . . ? C23 Si3 N3 Si4 41(2) . . . . ? C24 Si3 N3 Lu1 101.6(16) . . . . ? C23' Si3 N3 Lu1 -158(2) . . . . ? C24' Si3 N3 Lu1 67.9(16) . . . . ? C23 Si3 N3 Lu1 -143.8(19) . . . . ? N2 Lu1 N3 Si4 -140.8(6) . . . . ? N1 Lu1 N3 Si4 -33.7(7) . . . . ? C3 Lu1 N3 Si4 108.5(5) . . . . ? C2 Lu1 N3 Si4 119.4(6) . . . . ? C4 Lu1 N3 Si4 77.4(6) . . . . ? C1 Lu1 N3 Si4 81.3(9) . . . . ? C9 Lu1 N3 Si4 59.3(7) . . . . ? Si2 Lu1 N3 Si4 -110.9(5) . . . . ? N2 Lu1 N3 Si3 43.7(7) . . . . ? N1 Lu1 N3 Si3 150.7(6) . . . . ? C3 Lu1 N3 Si3 -67.0(7) . . . . ? C2 Lu1 N3 Si3 -56.1(9) . . . . ? C4 Lu1 N3 Si3 -98.2(7) . . . . ? C1 Lu1 N3 Si3 -94.3(9) . . . . ? C9 Lu1 N3 Si3 -116.3(7) . . . . ? Si2 Lu1 N3 Si3 73.6(7) . . . . ? Si4 Lu1 N3 Si3 -175.5(12) . . . . ? N3 Lu1 C1 C9 -40.5(15) . . . . ? N2 Lu1 C1 C9 -178.7(10) . . . . ? N1 Lu1 C1 C9 88.5(11) . . . . ? C3 Lu1 C1 C9 -75.3(10) . . . . ? C2 Lu1 C1 C9 -111.1(13) . . . . ? C4 Lu1 C1 C9 -35.5(9) . . . . ? Si2 Lu1 C1 C9 154.2(9) . . . . ? Si4 Lu1 C1 C9 1.0(13) . . . . ? N3 Lu1 C1 C2 70.6(10) . . . . ? N2 Lu1 C1 C2 -67.6(7) . . . . ? N1 Lu1 C1 C2 -160.4(8) . . . . ? C3 Lu1 C1 C2 35.8(7) . . . . ? C4 Lu1 C1 C2 75.6(7) . . . . ? C9 Lu1 C1 C2 111.1(13) . . . . ? Si2 Lu1 C1 C2 -94.6(7) . . . . ? Si4 Lu1 C1 C2 112.1(7) . . . . ? N3 Lu1 C1 C10 -171.7(9) . . . . ? N2 Lu1 C1 C10 50.1(10) . . . . ? N1 Lu1 C1 C10 -42.7(9) . . . . ? C3 Lu1 C1 C10 153.5(12) . . . . ? C2 Lu1 C1 C10 117.7(13) . . . . ? C4 Lu1 C1 C10 -166.7(12) . . . . ? C9 Lu1 C1 C10 -131.2(17) . . . . ? Si2 Lu1 C1 C10 23.0(11) . . . . ? Si4 Lu1 C1 C10 -130.2(9) . . . . ? C9 C1 C2 C3 2.1(17) . . . . ? C10 C1 C2 C3 179.9(12) . . . . ? Lu1 C1 C2 C3 -67.6(9) . . . . ? C9 C1 C2 Lu1 69.7(12) . . . . ? C10 C1 C2 Lu1 -112.5(13) . . . . ? N3 Lu1 C2 C3 -21.3(9) . . . . ? N2 Lu1 C2 C3 -128.6(7) . . . . ? N1 Lu1 C2 C3 135.5(6) . . . . ? C4 Lu1 C2 C3 38.4(6) . . . . ? C1 Lu1 C2 C3 115.6(11) . . . . ? C9 Lu1 C2 C3 77.8(8) . . . . ? Si2 Lu1 C2 C3 -137.6(6) . . . . ? Si4 Lu1 C2 C3 17.3(9) . . . . ? N3 Lu1 C2 C1 -136.9(7) . . . . ? N2 Lu1 C2 C1 115.8(7) . . . . ? N1 Lu1 C2 C1 19.9(8) . . . . ? C3 Lu1 C2 C1 -115.6(11) . . . . ? C4 Lu1 C2 C1 -77.1(9) . . . . ? C9 Lu1 C2 C1 -37.7(6) . . . . ? Si2 Lu1 C2 C1 106.9(7) . . . . ? Si4 Lu1 C2 C1 -98.2(7) . . . . ? C1 C2 C3 C4 -2.2(12) . . . . ? Lu1 C2 C3 C4 -71.2(7) . . . . ? C1 C2 C3 Lu1 69.0(9) . . . . ? N3 Lu1 C3 C2 162.6(7) . . . . ? N2 Lu1 C3 C2 55.5(7) . . . . ? N1 Lu1 C3 C2 -57.2(8) . . . . ? C4 Lu1 C3 C2 -111.7(8) . . . . ? C1 Lu1 C3 C2 -37.3(7) . . . . ? C9 Lu1 C3 C2 -76.4(8) . . . . ? Si2 Lu1 C3 C2 64.6(8) . . . . ? Si4 Lu1 C3 C2 -167.3(7) . . . . ? N3 Lu1 C3 C4 -85.7(7) . . . . ? N2 Lu1 C3 C4 167.2(7) . . . . ? N1 Lu1 C3 C4 54.5(8) . . . . ? C2 Lu1 C3 C4 111.7(8) . . . . ? C1 Lu1 C3 C4 74.4(8) . . . . ? C9 Lu1 C3 C4 35.3(7) . . . . ? Si2 Lu1 C3 C4 176.3(6) . . . . ? Si4 Lu1 C3 C4 -55.6(7) . . . . ? C2 C3 C4 C9 1.5(12) . . . . ? Lu1 C3 C4 C9 -67.7(10) . . . . ? C2 C3 C4 C5 -177.0(14) . . . . ? Lu1 C3 C4 C5 113.8(13) . . . . ? C2 C3 C4 Lu1 69.2(7) . . . . ? N3 Lu1 C4 C9 -147.0(8) . . . . ? N2 Lu1 C4 C9 98.0(9) . . . . ? N1 Lu1 C4 C9 -21.0(8) . . . . ? C3 Lu1 C4 C9 116.5(11) . . . . ? C2 Lu1 C4 C9 78.1(9) . . . . ? C1 Lu1 C4 C9 36.0(8) . . . . ? Si2 Lu1 C4 C9 100.9(19) . . . . ? Si4 Lu1 C4 C9 -116.8(8) . . . . ? N3 Lu1 C4 C3 96.5(7) . . . . ? N2 Lu1 C4 C3 -18.5(9) . . . . ? N1 Lu1 C4 C3 -137.5(6) . . . . ? C2 Lu1 C4 C3 -38.4(6) . . . . ? C1 Lu1 C4 C3 -80.6(8) . . . . ? C9 Lu1 C4 C3 -116.5(11) . . . . ? Si2 Lu1 C4 C3 -16(2) . . . . ? Si4 Lu1 C4 C3 126.6(6) . . . . ? N3 Lu1 C4 C5 -31.5(9) . . . . ? N2 Lu1 C4 C5 -146.5(8) . . . . ? N1 Lu1 C4 C5 94.5(9) . . . . ? C3 Lu1 C4 C5 -128.0(13) . . . . ? C2 Lu1 C4 C5 -166.4(12) . . . . ? C1 Lu1 C4 C5 151.4(11) . . . . ? C9 Lu1 C4 C5 115.5(13) . . . . ? Si2 Lu1 C4 C5 -143.6(15) . . . . ? Si4 Lu1 C4 C5 -1.4(9) . . . . ? C9 C4 C5 C6 -0.4(17) . . . . ? C3 C4 C5 C6 177.9(12) . . . . ? Lu1 C4 C5 C6 -91.0(11) . . . . ? C4 C5 C6 C7 1.7(17) . . . . ? C5 C6 C7 C8 0.1(19) . . . . ? C6 C7 C8 C9 -3(2) . . . . ? C7 C8 C9 C4 4(2) . . . . ? C7 C8 C9 C1 -176.9(18) . . . . ? C7 C8 C9 Lu1 89.8(14) . . . . ? C3 C4 C9 C8 178.9(12) . . . . ? C5 C4 C9 C8 -2.4(19) . . . . ? Lu1 C4 C9 C8 114.5(13) . . . . ? C3 C4 C9 C1 -0.1(18) . . . . ? C5 C4 C9 C1 178.6(13) . . . . ? Lu1 C4 C9 C1 -64.5(13) . . . . ? C3 C4 C9 Lu1 64.4(8) . . . . ? C5 C4 C9 Lu1 -116.9(11) . . . . ? C2 C1 C9 C8 -180.0(14) . . . . ? C10 C1 C9 C8 2(4) . . . . ? Lu1 C1 C9 C8 -114(2) . . . . ? C2 C1 C9 C4 -1(2) . . . . ? C10 C1 C9 C4 -178.7(13) . . . . ? Lu1 C1 C9 C4 64.6(11) . . . . ? C2 C1 C9 Lu1 -65.8(10) . . . . ? C10 C1 C9 Lu1 116.7(19) . . . . ? N3 Lu1 C9 C8 -75.9(12) . . . . ? N2 Lu1 C9 C8 131.7(10) . . . . ? N1 Lu1 C9 C8 45.7(11) . . . . ? C3 Lu1 C9 C8 -149.9(13) . . . . ? C2 Lu1 C9 C8 169.9(14) . . . . ? C4 Lu1 C9 C8 -113.6(15) . . . . ? C1 Lu1 C9 C8 129.9(18) . . . . ? Si2 Lu1 C9 C8 84.0(13) . . . . ? Si4 Lu1 C9 C8 -49.3(11) . . . . ? N3 Lu1 C9 C4 37.8(9) . . . . ? N2 Lu1 C9 C4 -114.7(8) . . . . ? N1 Lu1 C9 C4 159.3(8) . . . . ? C3 Lu1 C9 C4 -36.3(7) . . . . ? C2 Lu1 C9 C4 -76.5(8) . . . . ? C1 Lu1 C9 C4 -116.4(14) . . . . ? Si2 Lu1 C9 C4 -162.3(6) . . . . ? Si4 Lu1 C9 C4 64.4(8) . . . . ? N3 Lu1 C9 C1 154.2(10) . . . . ? N2 Lu1 C9 C1 1.7(14) . . . . ? N1 Lu1 C9 C1 -84.2(11) . . . . ? C3 Lu1 C9 C1 80.2(11) . . . . ? C2 Lu1 C9 C1 40.0(9) . . . . ? C4 Lu1 C9 C1 116.4(14) . . . . ? Si2 Lu1 C9 C1 -45.9(14) . . . . ? Si4 Lu1 C9 C1 -179.2(10) . . . . ? C9 C1 C10 C17 152.5(19) . . . . ? C2 C1 C10 C17 -24.6(18) . . . . ? Lu1 C1 C10 C17 -109.5(11) . . . . ? C9 C1 C10 C18 32(3) . . . . ? C2 C1 C10 C18 -145.0(13) . . . . ? Lu1 C1 C10 C18 130.1(10) . . . . ? C9 C1 C10 C11 -90(2) . . . . ? C2 C1 C10 C11 93.1(15) . . . . ? Lu1 C1 C10 C11 8.2(14) . . . . ? C1 C10 C11 C12 60.9(14) . . . . ? C17 C10 C11 C12 -178.6(10) . . . . ? C18 C10 C11 C12 -61.8(14) . . . . ? C16 N1 C12 C13 -1.4(17) . . . . ? Lu1 N1 C12 C13 -173.7(8) . . . . ? C16 N1 C12 C11 -174.5(10) . . . . ? Lu1 N1 C12 C11 13.2(14) . . . . ? C10 C11 C12 C13 106.5(13) . . . . ? C10 C11 C12 N1 -80.4(14) . . . . ? N1 C12 C13 C14 0.9(19) . . . . ? C11 C12 C13 C14 173.9(11) . . . . ? C12 C13 C14 C15 0.3(18) . . . . ? C13 C14 C15 C16 -0.9(16) . . . . ? C12 N1 C16 C15 0.8(16) . . . . ? Lu1 N1 C16 C15 173.6(8) . . . . ? C14 C15 C16 N1 0.3(17) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.196 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.103 data_shelxl5 _database_code_depnum_ccdc_archive 'CCDC 900284' #TrackingRef 'CCDC 900280.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H50 La N3 Si2, C6 H14' _chemical_formula_sum 'C46 H64 La N3 Si2' _chemical_formula_weight 854.09 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.005(2) _cell_length_b 15.948(3) _cell_length_c 13.217(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.872(4) _cell_angle_gamma 90.00 _cell_volume 2295.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9613 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.68 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 1.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.389 _exptl_absorpt_correction_T_max 0.627 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22001 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8268 _reflns_number_gt 7689 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.1922P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.042(13) _refine_ls_number_reflns 8268 _refine_ls_number_parameters 469 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.131 _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 La1 La 0.373290(15) 0.25246(2) 0.199884(14) 0.03905(7) Uani 1 1 d . . . Si1 Si 0.06958(12) 0.22786(8) -0.00661(12) 0.0636(4) Uani 1 1 d D . . H1 H 0.154(3) 0.227(3) -0.060(3) 0.070(14) Uiso 1 1 d D . . Si2 Si 0.07656(13) 0.28825(11) 0.20868(13) 0.0716(4) Uani 1 1 d D . . H2 H 0.157(3) 0.272(3) 0.3259(13) 0.072(15) Uiso 1 1 d D . . N1 N 0.3434(4) 0.1455(3) 0.3496(4) 0.0567(12) Uani 1 1 d . . . N2 N 0.3387(4) 0.3577(3) 0.0232(3) 0.0536(9) Uani 1 1 d . . . N3 N 0.1482(3) 0.2553(4) 0.1288(3) 0.0553(7) Uani 1 1 d . . . C1 C 0.4954(4) 0.3239(3) 0.4246(3) 0.0523(11) Uani 1 1 d . . . C2 C 0.3904(5) 0.3734(3) 0.3659(4) 0.0526(14) Uani 1 1 d . . . H2A H 0.3256 0.3846 0.3909 0.063 Uiso 1 1 calc R . . C3 C 0.4075(5) 0.4188(3) 0.2828(4) 0.0591(12) Uani 1 1 d . . . H3A H 0.3575 0.4669 0.2428 0.071 Uiso 1 1 calc R . . C4 C 0.5252(4) 0.4005(3) 0.2897(4) 0.0513(10) Uani 1 1 d . . . C5 C 0.5944(5) 0.4342(3) 0.2331(4) 0.0670(13) Uani 1 1 d . . . H5 H 0.5591 0.4729 0.1758 0.080 Uiso 1 1 calc R . . C6 C 0.7116(6) 0.4088(4) 0.2642(5) 0.0738(15) Uani 1 1 d . . . H6 H 0.7570 0.4308 0.2282 0.089 Uiso 1 1 calc R . . C7 C 0.7658(5) 0.3503(4) 0.3489(5) 0.0717(15) Uani 1 1 d . . . H7 H 0.8470 0.3347 0.3689 0.086 Uiso 1 1 calc R . . C8 C 0.7023(4) 0.3146(3) 0.4041(4) 0.0590(12) Uani 1 1 d . . . H8 H 0.7396 0.2741 0.4585 0.071 Uiso 1 1 calc R . . C9 C 0.5810(4) 0.3399(3) 0.3776(4) 0.0516(10) Uani 1 1 d . . . C10 C 0.5183(5) 0.2726(3) 0.5299(4) 0.0651(17) Uani 1 1 d . . . C11 C 0.5343(5) 0.1793(4) 0.5131(4) 0.0690(14) Uani 1 1 d . . . H11A H 0.5812 0.1739 0.4691 0.083 Uiso 1 1 calc R . . H11B H 0.5825 0.1544 0.5855 0.083 Uiso 1 1 calc R . . C12 C 0.4194(5) 0.1303(3) 0.4581(4) 0.0643(14) Uani 1 1 d . . . C13 C 0.3864(7) 0.0686(4) 0.5150(6) 0.0882(19) Uani 1 1 d . . . H13 H 0.4377 0.0573 0.5892 0.106 Uiso 1 1 calc R . . C14 C 0.2804(8) 0.0247(4) 0.4636(7) 0.101(2) Uani 1 1 d . . . H14 H 0.2587 -0.0157 0.5027 0.121 Uiso 1 1 calc R . . C15 C 0.2082(6) 0.0397(4) 0.3574(6) 0.0829(17) Uani 1 1 d . . . H15 H 0.1362 0.0093 0.3208 0.099 Uiso 1 1 calc R . . C16 C 0.2411(5) 0.1003(3) 0.3028(5) 0.0648(13) Uani 1 1 d . . . H16 H 0.1891 0.1107 0.2285 0.078 Uiso 1 1 calc R . . C17 C 0.4124(6) 0.2850(4) 0.5666(5) 0.0874(19) Uani 1 1 d . . . H17A H 0.3367 0.2659 0.5085 0.131 Uiso 1 1 calc R . . H17B H 0.4055 0.3434 0.5807 0.131 Uiso 1 1 calc R . . H17C H 0.4296 0.2534 0.6334 0.131 Uiso 1 1 calc R . . C18 C 0.6391(6) 0.3065(5) 0.6243(4) 0.098(2) Uani 1 1 d . . . H18A H 0.6541 0.2781 0.6928 0.147 Uiso 1 1 calc R . . H18B H 0.6311 0.3656 0.6334 0.147 Uiso 1 1 calc R . . H18C H 0.7064 0.2968 0.6046 0.147 Uiso 1 1 calc R . . C19 C 0.4821(4) 0.1782(3) 0.0610(3) 0.0456(9) Uani 1 1 d . . . C20 C 0.5784(4) 0.1923(3) 0.1680(4) 0.0506(10) Uani 1 1 d . . . H20A H 0.6519 0.2256 0.1816 0.061 Uiso 1 1 calc R . . C21 C 0.5680(4) 0.1367(3) 0.2446(4) 0.0528(11) Uani 1 1 d . . . H21A H 0.6332 0.1258 0.3189 0.063 Uiso 1 1 calc R . . C22 C 0.4686(4) 0.0823(3) 0.1876(4) 0.0494(10) Uani 1 1 d . . . C23 C 0.4236(5) 0.0116(3) 0.2221(5) 0.0630(13) Uani 1 1 d . . . H23 H 0.4584 -0.0047 0.2966 0.076 Uiso 1 1 calc R . . C24 C 0.3293(6) -0.0324(3) 0.1461(6) 0.0779(17) Uani 1 1 d . . . H24 H 0.3007 -0.0797 0.1689 0.094 Uiso 1 1 calc R . . C25 C 0.2739(5) -0.0087(3) 0.0343(5) 0.0708(14) Uani 1 1 d . . . H25 H 0.2090 -0.0402 -0.0159 0.085 Uiso 1 1 calc R . . C26 C 0.3132(5) 0.0600(3) -0.0024(4) 0.0614(12) Uani 1 1 d . . . H26 H 0.2740 0.0752 -0.0771 0.074 Uiso 1 1 calc R . . C27 C 0.4134(4) 0.1092(3) 0.0718(3) 0.0458(10) Uani 1 1 d . . . C28 C 0.4813(5) 0.2196(4) -0.0441(5) 0.0592(14) Uani 1 1 d . . . C29 C 0.5057(5) 0.3142(4) -0.0260(5) 0.0639(16) Uani 1 1 d . . . H29A H 0.5689 0.3223 0.0489 0.077 Uiso 1 1 calc R . . H29B H 0.5392 0.3332 -0.0772 0.077 Uiso 1 1 calc R . . C30 C 0.4005(5) 0.3697(3) -0.0400(4) 0.0627(13) Uani 1 1 d . . . C31 C 0.3676(7) 0.4339(4) -0.1177(6) 0.092(2) Uani 1 1 d . . . H31 H 0.4097 0.4412 -0.1622 0.111 Uiso 1 1 calc R . . C32 C 0.2727(8) 0.4869(4) -0.1290(6) 0.105(2) Uani 1 1 d . . . H32 H 0.2522 0.5312 -0.1793 0.126 Uiso 1 1 calc R . . C33 C 0.2090(7) 0.4741(4) -0.0663(5) 0.0853(18) Uani 1 1 d . . . H33 H 0.1435 0.5085 -0.0735 0.102 Uiso 1 1 calc R . . C34 C 0.2445(5) 0.4091(3) 0.0073(4) 0.0636(13) Uani 1 1 d . . . H34 H 0.2003 0.3998 0.0495 0.076 Uiso 1 1 calc R . . C35 C 0.3625(5) 0.2058(4) -0.1490(4) 0.0705(14) Uani 1 1 d . . . H35A H 0.3649 0.2381 -0.2094 0.106 Uiso 1 1 calc R . . H35B H 0.2938 0.2233 -0.1351 0.106 Uiso 1 1 calc R . . H35C H 0.3544 0.1474 -0.1685 0.106 Uiso 1 1 calc R . . C36 C 0.5865(5) 0.1811(4) -0.0648(5) 0.0819(17) Uani 1 1 d . . . H36A H 0.6636 0.1977 -0.0062 0.123 Uiso 1 1 calc R . . H36B H 0.5823 0.2004 -0.1351 0.123 Uiso 1 1 calc R . . H36C H 0.5798 0.1211 -0.0660 0.123 Uiso 1 1 calc R . . C37 C -0.0496(6) 0.3064(5) -0.0937(5) 0.105(2) Uani 1 1 d . . . H37A H -0.1109 0.3120 -0.0653 0.158 Uiso 1 1 calc R . . H37B H -0.0875 0.2874 -0.1696 0.158 Uiso 1 1 calc R . . H37C H -0.0111 0.3597 -0.0904 0.158 Uiso 1 1 calc R . . C38 C -0.0094(6) 0.1248(4) -0.0307(6) 0.095(2) Uani 1 1 d . . . H38A H 0.0489 0.0820 0.0086 0.143 Uiso 1 1 calc R . . H38B H -0.0455 0.1125 -0.1091 0.143 Uiso 1 1 calc R . . H38C H -0.0725 0.1268 -0.0042 0.143 Uiso 1 1 calc R . . C39 C 0.0417(7) 0.4017(5) 0.1955(7) 0.114(3) Uani 1 1 d . . . H39A H 0.1149 0.4327 0.2389 0.171 Uiso 1 1 calc R . . H39B H -0.0198 0.4134 0.2221 0.171 Uiso 1 1 calc R . . H39C H 0.0119 0.4180 0.1186 0.171 Uiso 1 1 calc R . . C40 C -0.0689(6) 0.2317(8) 0.1802(7) 0.154(5) Uani 1 1 d . . . H40A H -0.1266 0.2420 0.1047 0.231 Uiso 1 1 calc R . . H40B H -0.1024 0.2512 0.2303 0.231 Uiso 1 1 calc R . . H40C H -0.0528 0.1726 0.1909 0.231 Uiso 1 1 calc R . . C41 C 1.020(3) 0.232(2) 0.643(3) 0.270(6) Uiso 0.50 1 d PD A 1 H41A H 1.0120 0.2542 0.7073 0.405 Uiso 0.50 1 calc PR A 1 H41B H 0.9774 0.2676 0.5801 0.405 Uiso 0.50 1 calc PR A 1 H41C H 1.1052 0.2291 0.6576 0.405 Uiso 0.50 1 calc PR A 1 C42 C 0.965(4) 0.146(2) 0.619(3) 0.270(6) Uiso 0.50 1 d PD A 1 H42A H 0.8775 0.1453 0.5967 0.324 Uiso 0.50 1 calc PR A 1 H42B H 1.0063 0.1064 0.6790 0.324 Uiso 0.50 1 calc PR A 1 C43 C 1.001(4) 0.134(2) 0.519(3) 0.270(6) Uiso 0.50 1 d PD A 1 H43A H 0.9675 0.1782 0.4643 0.324 Uiso 0.50 1 calc PR A 1 H43B H 1.0886 0.1300 0.5435 0.324 Uiso 0.50 1 calc PR A 1 C44 C 0.938(4) 0.053(2) 0.479(4) 0.270(6) Uiso 0.50 1 d PD A 1 H44A H 1.0101 0.0173 0.5071 0.324 Uiso 0.50 1 calc PR A 1 H44B H 0.9202 0.0599 0.4006 0.324 Uiso 0.50 1 calc PR A 1 C45 C 0.844(4) -0.012(2) 0.467(4) 0.270(6) Uiso 0.50 1 d PD A 1 H45A H 0.7633 0.0032 0.4103 0.324 Uiso 0.50 1 calc PR A 1 H45B H 0.8382 -0.0225 0.5369 0.324 Uiso 0.50 1 calc PR A 1 C46 C 0.898(4) -0.087(2) 0.431(3) 0.270(6) Uiso 0.50 1 d PD A 1 H46A H 0.8468 -0.1355 0.4206 0.405 Uiso 0.50 1 calc PR A 1 H46B H 0.9790 -0.0990 0.4869 0.405 Uiso 0.50 1 calc PR A 1 H46C H 0.9031 -0.0744 0.3616 0.405 Uiso 0.50 1 calc PR A 1 C41' C 1.085(4) 0.299(2) 0.599(3) 0.270(6) Uiso 0.50 1 d PD B 2 H41D H 1.1067 0.3348 0.5514 0.405 Uiso 0.50 1 calc PR B 2 H41E H 1.1471 0.3021 0.6736 0.405 Uiso 0.50 1 calc PR B 2 H41F H 1.0077 0.3170 0.5969 0.405 Uiso 0.50 1 calc PR B 2 C42' C 1.073(4) 0.209(2) 0.557(3) 0.270(6) Uiso 0.50 1 d PD B 2 H42C H 1.0143 0.2061 0.4797 0.324 Uiso 0.50 1 calc PR B 2 H42D H 1.1519 0.1892 0.5628 0.324 Uiso 0.50 1 calc PR B 2 C43' C 1.032(4) 0.160(2) 0.627(3) 0.270(6) Uiso 0.50 1 d PD B 2 H43C H 0.9719 0.1905 0.6433 0.324 Uiso 0.50 1 calc PR B 2 H43D H 1.1011 0.1462 0.6972 0.324 Uiso 0.50 1 calc PR B 2 C44' C 0.974(3) 0.078(2) 0.562(3) 0.270(6) Uiso 0.50 1 d PD B 2 H44C H 0.9503 0.0827 0.4822 0.324 Uiso 0.50 1 calc PR B 2 H44D H 1.0257 0.0287 0.5913 0.324 Uiso 0.50 1 calc PR B 2 C45' C 0.865(3) 0.081(2) 0.593(3) 0.270(6) Uiso 0.50 1 d PD B 2 H45C H 0.8866 0.0648 0.6699 0.324 Uiso 0.50 1 calc PR B 2 H45D H 0.8245 0.1355 0.5783 0.324 Uiso 0.50 1 calc PR B 2 C46' C 0.793(3) 0.016(2) 0.511(3) 0.270(6) Uiso 0.50 1 d PD B 2 H46D H 0.7155 0.0073 0.5157 0.405 Uiso 0.50 1 calc PR B 2 H46E H 0.8378 -0.0359 0.5280 0.405 Uiso 0.50 1 calc PR B 2 H46F H 0.7777 0.0336 0.4373 0.405 Uiso 0.50 1 calc PR B 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 La1 0.03796(11) 0.04617(12) 0.03376(10) 0.00012(13) 0.01580(8) 0.00090(14) Si1 0.0479(7) 0.0763(12) 0.0618(8) -0.0025(6) 0.0182(6) -0.0023(6) Si2 0.0479(7) 0.0960(10) 0.0714(9) -0.0087(7) 0.0254(7) 0.0019(7) N1 0.065(3) 0.059(3) 0.054(3) 0.010(2) 0.033(2) 0.013(2) N2 0.055(2) 0.063(2) 0.043(2) 0.0034(17) 0.0206(19) -0.007(2) N3 0.0424(16) 0.0645(19) 0.0577(18) 0.006(3) 0.0198(14) 0.004(3) C1 0.054(3) 0.064(3) 0.035(2) -0.0121(19) 0.015(2) 0.001(2) C2 0.056(3) 0.061(3) 0.041(3) -0.016(2) 0.021(2) 0.010(2) C3 0.061(3) 0.051(3) 0.053(3) -0.010(2) 0.013(2) 0.007(2) C4 0.054(3) 0.050(2) 0.046(3) -0.0083(19) 0.016(2) -0.004(2) C5 0.080(4) 0.066(3) 0.052(3) -0.010(2) 0.025(3) -0.011(3) C6 0.067(4) 0.081(4) 0.078(4) -0.017(3) 0.035(3) -0.021(3) C7 0.048(3) 0.094(4) 0.071(4) -0.034(3) 0.023(3) -0.015(3) C8 0.052(3) 0.065(3) 0.052(3) -0.014(2) 0.014(2) -0.003(2) C9 0.049(2) 0.057(3) 0.043(2) -0.0133(19) 0.013(2) -0.005(2) C10 0.073(3) 0.088(5) 0.036(2) 0.002(2) 0.025(2) 0.011(3) C11 0.074(4) 0.085(4) 0.042(3) 0.015(3) 0.019(3) 0.017(3) C12 0.088(4) 0.058(3) 0.056(3) 0.020(2) 0.039(3) 0.025(3) C13 0.110(5) 0.086(4) 0.075(4) 0.037(3) 0.045(4) 0.016(4) C14 0.125(6) 0.085(4) 0.114(6) 0.043(4) 0.072(5) 0.005(4) C15 0.089(4) 0.075(4) 0.101(5) 0.029(3) 0.055(4) 0.011(3) C16 0.069(3) 0.056(3) 0.074(3) 0.006(2) 0.035(3) 0.005(3) C17 0.112(5) 0.103(5) 0.065(3) -0.004(3) 0.054(3) 0.015(3) C18 0.104(5) 0.133(5) 0.036(3) -0.008(3) 0.009(3) -0.003(4) C19 0.050(2) 0.050(2) 0.042(2) -0.0060(17) 0.026(2) -0.0016(19) C20 0.043(2) 0.064(3) 0.049(3) -0.013(2) 0.024(2) -0.004(2) C21 0.047(3) 0.062(3) 0.044(3) -0.006(2) 0.015(2) 0.007(2) C22 0.057(3) 0.047(2) 0.052(3) 0.0006(19) 0.030(2) 0.011(2) C23 0.081(4) 0.052(3) 0.067(3) -0.001(2) 0.043(3) 0.006(3) C24 0.100(4) 0.055(3) 0.102(5) -0.005(3) 0.065(4) -0.008(3) C25 0.065(3) 0.061(3) 0.082(4) -0.015(3) 0.027(3) -0.020(3) C26 0.063(3) 0.068(3) 0.051(3) -0.010(2) 0.021(2) -0.006(3) C27 0.047(2) 0.053(3) 0.041(2) -0.0077(19) 0.022(2) -0.002(2) C28 0.065(3) 0.075(3) 0.048(3) -0.002(2) 0.034(2) -0.008(2) C29 0.061(3) 0.078(4) 0.065(4) 0.015(3) 0.039(3) -0.005(3) C30 0.076(3) 0.061(3) 0.056(3) 0.001(2) 0.032(3) -0.018(3) C31 0.136(6) 0.067(4) 0.103(5) 0.025(3) 0.079(5) -0.006(4) C32 0.154(7) 0.065(4) 0.113(5) 0.038(4) 0.073(5) 0.015(4) C33 0.105(5) 0.068(4) 0.088(4) 0.023(3) 0.045(4) 0.012(3) C34 0.071(3) 0.063(3) 0.053(3) 0.004(2) 0.024(3) -0.003(3) C35 0.084(4) 0.088(3) 0.043(3) 0.000(2) 0.029(3) -0.005(3) C36 0.085(4) 0.112(5) 0.072(4) 0.003(3) 0.056(3) 0.011(3) C37 0.083(4) 0.114(5) 0.076(4) 0.004(4) -0.009(3) 0.012(4) C38 0.080(4) 0.094(5) 0.104(5) -0.027(4) 0.031(4) -0.027(4) C39 0.093(5) 0.122(6) 0.112(6) -0.011(5) 0.027(4) 0.051(4) C40 0.089(4) 0.262(15) 0.147(6) -0.068(9) 0.085(5) -0.073(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 N3 2.460(3) . ? La1 N1 2.749(5) . ? La1 N2 2.762(4) . ? La1 C3 2.833(5) . ? La1 C20 2.834(4) . ? La1 C21 2.838(5) . ? La1 C2 2.864(5) . ? La1 C4 2.913(4) . ? La1 C19 2.914(4) . ? La1 C1 2.933(4) . ? La1 C9 2.958(4) . ? La1 C22 2.976(4) . ? Si1 N3 1.692(4) . ? Si1 C38 1.856(6) . ? Si1 C37 1.885(6) . ? Si1 H1 1.460(10) . ? Si2 N3 1.701(4) . ? Si2 C39 1.849(7) . ? Si2 C40 1.858(7) . ? Si2 H2 1.464(10) . ? N1 C16 1.331(7) . ? N1 C12 1.359(7) . ? N2 C34 1.339(7) . ? N2 C30 1.344(6) . ? C1 C2 1.411(7) . ? C1 C9 1.429(6) . ? C1 C10 1.537(6) . ? C2 C3 1.401(8) . ? C2 H2A 0.9800 . ? C3 C4 1.408(7) . ? C3 H3A 0.9800 . ? C4 C5 1.436(7) . ? C4 C9 1.442(6) . ? C5 C6 1.351(8) . ? C5 H5 0.9300 . ? C6 C7 1.391(8) . ? C6 H6 0.9300 . ? C7 C8 1.380(7) . ? C7 H7 0.9300 . ? C8 C9 1.406(6) . ? C8 H8 0.9300 . ? C10 C11 1.528(8) . ? C10 C17 1.552(7) . ? C10 C18 1.559(8) . ? C11 C12 1.482(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.393(7) . ? C13 C14 1.358(10) . ? C13 H13 0.9300 . ? C14 C15 1.325(10) . ? C14 H14 0.9300 . ? C15 C16 1.360(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.418(6) . ? C19 C27 1.418(6) . ? C19 C28 1.536(7) . ? C20 C21 1.390(7) . ? C20 H20A 0.9800 . ? C21 C22 1.410(6) . ? C21 H21A 0.9800 . ? C22 C23 1.406(7) . ? C22 C27 1.454(6) . ? C23 C24 1.352(8) . ? C23 H23 0.9300 . ? C24 C25 1.393(9) . ? C24 H24 0.9300 . ? C25 C26 1.361(7) . ? C25 H25 0.9300 . ? C26 C27 1.424(6) . ? C26 H26 0.9300 . ? C28 C36 1.529(7) . ? C28 C35 1.530(8) . ? C28 C29 1.535(8) . ? C29 C30 1.489(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.386(7) . ? C31 C32 1.375(9) . ? C31 H31 0.9300 . ? C32 C33 1.359(9) . ? C32 H32 0.9300 . ? C33 C34 1.362(8) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.496(19) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.549(19) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.473(19) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.498(19) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.538(18) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C41' C42' 1.516(18) . ? C41' H41D 0.9600 . ? C41' H41E 0.9600 . ? C41' H41F 0.9600 . ? C42' C43' 1.456(19) . ? C42' H42C 0.9700 . ? C42' H42D 0.9700 . ? C43' C44' 1.559(19) . ? C43' H43C 0.9700 . ? C43' H43D 0.9700 . ? C44' C45' 1.537(19) . ? C44' H44C 0.9700 . ? C44' H44D 0.9700 . ? C45' C46' 1.494(19) . ? C45' H45C 0.9700 . ? C45' H45D 0.9700 . ? C46' H46D 0.9600 . ? C46' H46E 0.9600 . ? C46' H46F 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 La1 N1 80.30(14) . . ? N3 La1 N2 85.14(13) . . ? N1 La1 N2 165.33(12) . . ? N3 La1 C3 95.02(17) . . ? N1 La1 C3 110.15(15) . . ? N2 La1 C3 72.75(13) . . ? N3 La1 C20 146.40(13) . . ? N1 La1 C20 106.36(13) . . ? N2 La1 C20 84.90(13) . . ? C3 La1 C20 112.37(14) . . ? N3 La1 C21 140.14(17) . . ? N1 La1 C21 77.99(14) . . ? N2 La1 C21 112.90(13) . . ? C3 La1 C21 123.76(14) . . ? C20 La1 C21 28.38(13) . . ? N3 La1 C2 89.63(15) . . ? N1 La1 C2 81.70(13) . . ? N2 La1 C2 100.08(16) . . ? C3 La1 C2 28.47(15) . . ? C20 La1 C2 123.71(14) . . ? C21 La1 C2 119.42(14) . . ? N3 La1 C4 122.65(17) . . ? N1 La1 C4 117.30(14) . . ? N2 La1 C4 72.40(12) . . ? C3 La1 C4 28.32(14) . . ? C20 La1 C4 84.30(13) . . ? C21 La1 C4 97.04(14) . . ? C2 La1 C4 46.44(15) . . ? N3 La1 C19 118.57(12) . . ? N1 La1 C19 115.46(12) . . ? N2 La1 C19 70.28(12) . . ? C3 La1 C19 126.41(14) . . ? C20 La1 C19 28.52(12) . . ? C21 La1 C19 47.07(13) . . ? C2 La1 C19 148.17(14) . . ? C4 La1 C19 102.50(13) . . ? N3 La1 C1 112.37(13) . . ? N1 La1 C1 70.93(14) . . ? N2 La1 C1 116.95(13) . . ? C3 La1 C1 46.80(14) . . ? C20 La1 C1 100.74(12) . . ? C21 La1 C1 91.41(13) . . ? C2 La1 C1 28.15(14) . . ? C4 La1 C1 46.53(13) . . ? C19 La1 C1 129.04(12) . . ? N3 La1 C9 135.91(14) . . ? N1 La1 C9 92.44(14) . . ? N2 La1 C9 99.30(12) . . ? C3 La1 C9 46.78(13) . . ? C20 La1 C9 77.45(12) . . ? C21 La1 C9 78.22(13) . . ? C2 La1 C9 46.31(14) . . ? C4 La1 C9 28.41(13) . . ? C19 La1 C9 103.90(12) . . ? C1 La1 C9 28.07(12) . . ? N3 La1 C22 112.45(17) . . ? N1 La1 C22 69.06(12) . . ? N2 La1 C22 115.65(12) . . ? C3 La1 C22 151.45(13) . . ? C20 La1 C22 46.01(13) . . ? C21 La1 C22 27.94(13) . . ? C2 La1 C22 138.66(14) . . ? C4 La1 C22 124.89(13) . . ? C19 La1 C22 46.43(12) . . ? C1 La1 C22 111.68(13) . . ? C9 La1 C22 104.95(13) . . ? N3 Si1 C38 115.3(3) . . ? N3 Si1 C37 114.6(3) . . ? C38 Si1 C37 106.3(3) . . ? N3 Si1 La1 38.79(10) . . ? C38 Si1 La1 121.1(2) . . ? C37 Si1 La1 131.9(2) . . ? N3 Si1 H1 108.7(17) . . ? C38 Si1 H1 108.8(18) . . ? C37 Si1 H1 102.2(17) . . ? La1 Si1 H1 70.9(17) . . ? N3 Si2 C39 113.4(3) . . ? N3 Si2 C40 113.7(3) . . ? C39 Si2 C40 107.4(5) . . ? N3 Si2 H2 108.7(17) . . ? C39 Si2 H2 107(2) . . ? C40 Si2 H2 106.0(17) . . ? C16 N1 C12 118.2(5) . . ? C16 N1 La1 112.1(3) . . ? C12 N1 La1 129.6(4) . . ? C34 N2 C30 117.8(4) . . ? C34 N2 La1 108.8(3) . . ? C30 N2 La1 133.3(3) . . ? Si1 N3 Si2 122.28(18) . . ? Si1 N3 La1 115.68(16) . . ? Si2 N3 La1 121.95(18) . . ? C2 C1 C9 107.5(4) . . ? C2 C1 C10 125.0(4) . . ? C9 C1 C10 126.9(4) . . ? C2 C1 La1 73.2(3) . . ? C9 C1 La1 76.9(2) . . ? C10 C1 La1 122.2(3) . . ? C3 C2 C1 109.2(5) . . ? C3 C2 La1 74.5(3) . . ? C1 C2 La1 78.7(3) . . ? C3 C2 H2A 124.7 . . ? C1 C2 H2A 124.7 . . ? La1 C2 H2A 124.7 . . ? C2 C3 C4 108.4(4) . . ? C2 C3 La1 77.0(3) . . ? C4 C3 La1 79.0(3) . . ? C2 C3 H3A 124.6 . . ? C4 C3 H3A 124.6 . . ? La1 C3 H3A 124.6 . . ? C3 C4 C5 132.3(5) . . ? C3 C4 C9 107.8(4) . . ? C5 C4 C9 119.8(5) . . ? C3 C4 La1 72.7(3) . . ? C5 C4 La1 119.4(3) . . ? C9 C4 La1 77.5(2) . . ? C6 C5 C4 119.0(5) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C7 121.4(5) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C6 121.8(5) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C7 C8 C9 119.7(5) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C8 C9 C1 134.4(5) . . ? C8 C9 C4 118.3(4) . . ? C1 C9 C4 107.1(4) . . ? C8 C9 La1 120.1(3) . . ? C1 C9 La1 75.0(2) . . ? C4 C9 La1 74.0(2) . . ? C11 C10 C1 111.9(4) . . ? C11 C10 C17 109.8(5) . . ? C1 C10 C17 110.9(4) . . ? C11 C10 C18 108.8(5) . . ? C1 C10 C18 107.0(5) . . ? C17 C10 C18 108.3(4) . . ? C12 C11 C10 115.9(5) . . ? C12 C11 H11A 108.3 . . ? C10 C11 H11A 108.3 . . ? C12 C11 H11B 108.3 . . ? C10 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? N1 C12 C13 118.6(6) . . ? N1 C12 C11 119.8(4) . . ? C13 C12 C11 121.6(5) . . ? C14 C13 C12 120.9(6) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C15 C14 C13 119.6(6) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 119.0(7) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? N1 C16 C15 123.7(6) . . ? N1 C16 H16 118.2 . . ? C15 C16 H16 118.2 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 C18 H18A 109.5 . . ? C10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C10 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C27 106.7(4) . . ? C20 C19 C28 121.7(4) . . ? C27 C19 C28 130.0(4) . . ? C20 C19 La1 72.6(2) . . ? C27 C19 La1 79.6(2) . . ? C28 C19 La1 124.2(3) . . ? C21 C20 C19 109.8(4) . . ? C21 C20 La1 76.0(2) . . ? C19 C20 La1 78.9(2) . . ? C21 C20 H20A 124.2 . . ? C19 C20 H20A 124.2 . . ? La1 C20 H20A 124.2 . . ? C20 C21 C22 108.6(4) . . ? C20 C21 La1 75.6(3) . . ? C22 C21 La1 81.5(3) . . ? C20 C21 H21A 124.4 . . ? C22 C21 H21A 124.4 . . ? La1 C21 H21A 124.4 . . ? C23 C22 C21 132.4(5) . . ? C23 C22 C27 120.7(4) . . ? C21 C22 C27 106.8(4) . . ? C23 C22 La1 120.3(3) . . ? C21 C22 La1 70.6(2) . . ? C27 C22 La1 76.9(2) . . ? C24 C23 C22 119.4(5) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 121.6(5) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C26 C25 C24 120.9(5) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 121.1(5) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C19 C27 C26 135.8(4) . . ? C19 C27 C22 107.9(4) . . ? C26 C27 C22 116.2(4) . . ? C19 C27 La1 72.7(2) . . ? C26 C27 La1 121.2(3) . . ? C22 C27 La1 75.0(2) . . ? C36 C28 C35 107.8(5) . . ? C36 C28 C29 107.7(5) . . ? C35 C28 C29 109.1(5) . . ? C36 C28 C19 107.3(4) . . ? C35 C28 C19 114.0(4) . . ? C29 C28 C19 110.7(5) . . ? C30 C29 C28 117.9(5) . . ? C30 C29 H29A 107.8 . . ? C28 C29 H29A 107.8 . . ? C30 C29 H29B 107.8 . . ? C28 C29 H29B 107.8 . . ? H29A C29 H29B 107.2 . . ? N2 C30 C31 120.4(5) . . ? N2 C30 C29 120.0(4) . . ? C31 C30 C29 119.6(5) . . ? C32 C31 C30 120.0(6) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 119.7(6) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 117.6(6) . . ? C32 C33 H33 121.2 . . ? C34 C33 H33 121.2 . . ? N2 C34 C33 124.6(6) . . ? N2 C34 H34 117.7 . . ? C33 C34 H34 117.7 . . ? C28 C35 H35A 109.5 . . ? C28 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C28 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C28 C36 H36A 109.5 . . ? C28 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C28 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si1 C37 H37A 109.5 . . ? Si1 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si1 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si1 C38 H38A 109.5 . . ? Si1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si2 C39 H39A 109.5 . . ? Si2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si2 C40 H40A 109.5 . . ? Si2 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si2 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C41 C42 C43 93(2) . . ? C41 C42 H42A 113.2 . . ? C43 C42 H42A 113.2 . . ? C41 C42 H42B 113.2 . . ? C43 C42 H42B 113.2 . . ? H42A C42 H42B 110.5 . . ? C44 C43 C42 98(3) . . ? C44 C43 H43A 112.2 . . ? C42 C43 H43A 112.2 . . ? C44 C43 H43B 112.2 . . ? C42 C43 H43B 112.2 . . ? H43A C43 H43B 109.8 . . ? C43 C44 C45 153(4) . . ? C43 C44 H44A 98.2 . . ? C45 C44 H44A 98.2 . . ? C43 C44 H44B 98.2 . . ? C45 C44 H44B 98.2 . . ? H44A C44 H44B 103.8 . . ? C44 C45 C46 100(3) . . ? C44 C45 H45A 111.8 . . ? C46 C45 H45A 111.8 . . ? C44 C45 H45B 111.8 . . ? C46 C45 H45B 111.8 . . ? H45A C45 H45B 109.5 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C42' C41' H41D 109.5 . . ? C42' C41' H41E 109.5 . . ? H41D C41' H41E 109.5 . . ? C42' C41' H41F 109.5 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? C43' C42' C41' 107(2) . . ? C43' C42' H42C 110.4 . . ? C41' C42' H42C 110.4 . . ? C43' C42' H42D 110.4 . . ? C41' C42' H42D 110.4 . . ? H42C C42' H42D 108.6 . . ? C42' C43' C44' 107(2) . . ? C42' C43' H43C 110.3 . . ? C44' C43' H43C 110.3 . . ? C42' C43' H43D 110.3 . . ? C44' C43' H43D 110.3 . . ? H43C C43' H43D 108.5 . . ? C45' C44' C43' 93(2) . . ? C45' C44' H44C 113.1 . . ? C43' C44' H44C 113.1 . . ? C45' C44' H44D 113.1 . . ? C43' C44' H44D 113.1 . . ? H44C C44' H44D 110.5 . . ? C46' C45' C44' 95(2) . . ? C46' C45' H45C 112.8 . . ? C44' C45' H45C 112.8 . . ? C46' C45' H45D 112.8 . . ? C44' C45' H45D 112.8 . . ? H45C C45' H45D 110.3 . . ? C45' C46' H46D 109.5 . . ? C45' C46' H46E 109.5 . . ? H46D C46' H46E 109.5 . . ? C45' C46' H46F 109.5 . . ? H46D C46' H46F 109.5 . . ? H46E C46' H46F 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 N1 La1 Si1 N3 55.6(3) . . . . ? N2 La1 Si1 N3 -120.7(3) . . . . ? C3 La1 Si1 N3 -57.8(3) . . . . ? C20 La1 Si1 N3 168.1(3) . . . . ? C21 La1 Si1 N3 134.2(3) . . . . ? C2 La1 Si1 N3 -27.4(4) . . . . ? C4 La1 Si1 N3 -78.4(3) . . . . ? C19 La1 Si1 N3 171.5(3) . . . . ? C1 La1 Si1 N3 -11.1(4) . . . . ? C9 La1 Si1 N3 -51.5(4) . . . . ? C22 La1 Si1 N3 125.1(3) . . . . ? N3 La1 Si1 C38 -92.7(4) . . . . ? N1 La1 Si1 C38 -37.1(3) . . . . ? N2 La1 Si1 C38 146.6(3) . . . . ? C3 La1 Si1 C38 -150.5(3) . . . . ? C20 La1 Si1 C38 75.4(3) . . . . ? C21 La1 Si1 C38 41.5(3) . . . . ? C2 La1 Si1 C38 -120.1(3) . . . . ? C4 La1 Si1 C38 -171.0(3) . . . . ? C19 La1 Si1 C38 78.8(3) . . . . ? C1 La1 Si1 C38 -103.8(3) . . . . ? C9 La1 Si1 C38 -144.2(3) . . . . ? C22 La1 Si1 C38 32.4(3) . . . . ? N3 La1 Si1 C37 77.0(5) . . . . ? N1 La1 Si1 C37 132.6(3) . . . . ? N2 La1 Si1 C37 -43.7(3) . . . . ? C3 La1 Si1 C37 19.2(4) . . . . ? C20 La1 Si1 C37 -114.9(4) . . . . ? C21 La1 Si1 C37 -148.8(4) . . . . ? C2 La1 Si1 C37 49.6(4) . . . . ? C4 La1 Si1 C37 -1.4(4) . . . . ? C19 La1 Si1 C37 -111.5(3) . . . . ? C1 La1 Si1 C37 65.9(4) . . . . ? C9 La1 Si1 C37 25.5(4) . . . . ? C22 La1 Si1 C37 -157.9(3) . . . . ? N3 La1 N1 C16 34.3(4) . . . . ? N2 La1 N1 C16 27.2(8) . . . . ? C3 La1 N1 C16 126.1(3) . . . . ? C20 La1 N1 C16 -111.9(3) . . . . ? C21 La1 N1 C16 -112.1(4) . . . . ? C2 La1 N1 C16 125.3(3) . . . . ? C4 La1 N1 C16 156.1(3) . . . . ? C19 La1 N1 C16 -82.9(4) . . . . ? C1 La1 N1 C16 152.1(4) . . . . ? C9 La1 N1 C16 170.5(4) . . . . ? C22 La1 N1 C16 -84.4(4) . . . . ? N3 La1 N1 C12 -149.7(4) . . . . ? N2 La1 N1 C12 -156.7(5) . . . . ? C3 La1 N1 C12 -57.8(4) . . . . ? C20 La1 N1 C12 64.2(4) . . . . ? C21 La1 N1 C12 64.0(4) . . . . ? C2 La1 N1 C12 -58.6(4) . . . . ? C4 La1 N1 C12 -27.8(5) . . . . ? C19 La1 N1 C12 93.2(4) . . . . ? C1 La1 N1 C12 -31.8(4) . . . . ? C9 La1 N1 C12 -13.4(4) . . . . ? C22 La1 N1 C12 91.6(4) . . . . ? N3 La1 N2 C34 36.0(3) . . . . ? N1 La1 N2 C34 43.0(7) . . . . ? C3 La1 N2 C34 -60.8(3) . . . . ? C20 La1 N2 C34 -176.1(3) . . . . ? C21 La1 N2 C34 179.2(3) . . . . ? C2 La1 N2 C34 -52.7(3) . . . . ? C4 La1 N2 C34 -90.5(3) . . . . ? C19 La1 N2 C34 158.7(4) . . . . ? C1 La1 N2 C34 -76.6(4) . . . . ? C9 La1 N2 C34 -99.7(3) . . . . ? C22 La1 N2 C34 148.6(3) . . . . ? N3 La1 N2 C30 -149.2(5) . . . . ? N1 La1 N2 C30 -142.2(5) . . . . ? C3 La1 N2 C30 114.0(5) . . . . ? C20 La1 N2 C30 -1.3(4) . . . . ? C21 La1 N2 C30 -6.0(5) . . . . ? C2 La1 N2 C30 122.1(4) . . . . ? C4 La1 N2 C30 84.3(4) . . . . ? C19 La1 N2 C30 -26.5(4) . . . . ? C1 La1 N2 C30 98.2(4) . . . . ? C9 La1 N2 C30 75.0(4) . . . . ? C22 La1 N2 C30 -36.6(5) . . . . ? C38 Si1 N3 Si2 -74.5(5) . . . . ? C37 Si1 N3 Si2 49.4(5) . . . . ? La1 Si1 N3 Si2 176.6(6) . . . . ? C38 Si1 N3 La1 108.9(3) . . . . ? C37 Si1 N3 La1 -127.2(4) . . . . ? C39 Si2 N3 Si1 -85.4(5) . . . . ? C40 Si2 N3 Si1 37.7(6) . . . . ? C39 Si2 N3 La1 91.0(4) . . . . ? C40 Si2 N3 La1 -145.9(5) . . . . ? N1 La1 N3 Si1 -123.5(3) . . . . ? N2 La1 N3 Si1 54.7(3) . . . . ? C3 La1 N3 Si1 126.9(3) . . . . ? C20 La1 N3 Si1 -18.5(5) . . . . ? C21 La1 N3 Si1 -65.8(4) . . . . ? C2 La1 N3 Si1 154.9(3) . . . . ? C4 La1 N3 Si1 120.2(3) . . . . ? C19 La1 N3 Si1 -9.7(4) . . . . ? C1 La1 N3 Si1 171.9(3) . . . . ? C9 La1 N3 Si1 153.1(2) . . . . ? C22 La1 N3 Si1 -61.1(3) . . . . ? N1 La1 N3 Si2 59.9(3) . . . . ? N2 La1 N3 Si2 -121.9(3) . . . . ? C3 La1 N3 Si2 -49.7(3) . . . . ? C20 La1 N3 Si2 164.9(2) . . . . ? C21 La1 N3 Si2 117.6(3) . . . . ? C2 La1 N3 Si2 -21.7(3) . . . . ? C4 La1 N3 Si2 -56.4(4) . . . . ? C19 La1 N3 Si2 173.7(3) . . . . ? C1 La1 N3 Si2 -4.7(4) . . . . ? C9 La1 N3 Si2 -23.5(5) . . . . ? C22 La1 N3 Si2 122.3(3) . . . . ? N3 La1 C1 C2 -38.4(4) . . . . ? N1 La1 C1 C2 -108.8(3) . . . . ? N2 La1 C1 C2 57.7(3) . . . . ? C3 La1 C1 C2 36.8(3) . . . . ? C20 La1 C1 C2 147.4(3) . . . . ? C21 La1 C1 C2 174.4(3) . . . . ? C4 La1 C1 C2 76.1(3) . . . . ? C19 La1 C1 C2 143.4(3) . . . . ? C9 La1 C1 C2 113.1(4) . . . . ? C22 La1 C1 C2 -165.8(3) . . . . ? N3 La1 C1 C9 -151.5(3) . . . . ? N1 La1 C1 C9 138.1(3) . . . . ? N2 La1 C1 C9 -55.4(3) . . . . ? C3 La1 C1 C9 -76.4(3) . . . . ? C20 La1 C1 C9 34.3(3) . . . . ? C21 La1 C1 C9 61.3(3) . . . . ? C2 La1 C1 C9 -113.1(4) . . . . ? C4 La1 C1 C9 -37.1(3) . . . . ? C19 La1 C1 C9 30.3(3) . . . . ? C22 La1 C1 C9 81.1(3) . . . . ? N3 La1 C1 C10 82.8(4) . . . . ? N1 La1 C1 C10 12.4(3) . . . . ? N2 La1 C1 C10 178.9(3) . . . . ? C3 La1 C1 C10 158.0(4) . . . . ? C20 La1 C1 C10 -91.4(4) . . . . ? C21 La1 C1 C10 -64.4(4) . . . . ? C2 La1 C1 C10 121.2(5) . . . . ? C4 La1 C1 C10 -162.7(4) . . . . ? C19 La1 C1 C10 -95.4(4) . . . . ? C9 La1 C1 C10 -125.7(5) . . . . ? C22 La1 C1 C10 -44.6(4) . . . . ? C9 C1 C2 C3 0.9(5) . . . . ? C10 C1 C2 C3 173.0(4) . . . . ? La1 C1 C2 C3 -69.1(3) . . . . ? C9 C1 C2 La1 70.0(3) . . . . ? C10 C1 C2 La1 -117.9(4) . . . . ? N3 La1 C2 C3 -101.3(3) . . . . ? N1 La1 C2 C3 178.5(3) . . . . ? N2 La1 C2 C3 -16.3(3) . . . . ? C20 La1 C2 C3 74.3(3) . . . . ? C21 La1 C2 C3 107.4(3) . . . . ? C4 La1 C2 C3 37.4(3) . . . . ? C19 La1 C2 C3 52.4(4) . . . . ? C1 La1 C2 C3 113.8(5) . . . . ? C9 La1 C2 C3 77.0(3) . . . . ? C22 La1 C2 C3 133.9(3) . . . . ? N3 La1 C2 C1 145.0(3) . . . . ? N1 La1 C2 C1 64.7(3) . . . . ? N2 La1 C2 C1 -130.0(3) . . . . ? C3 La1 C2 C1 -113.8(5) . . . . ? C20 La1 C2 C1 -39.5(4) . . . . ? C21 La1 C2 C1 -6.4(4) . . . . ? C4 La1 C2 C1 -76.4(3) . . . . ? C19 La1 C2 C1 -61.4(4) . . . . ? C9 La1 C2 C1 -36.8(3) . . . . ? C22 La1 C2 C1 20.2(4) . . . . ? C1 C2 C3 C4 -1.7(5) . . . . ? La1 C2 C3 C4 -73.5(3) . . . . ? C1 C2 C3 La1 71.8(3) . . . . ? N3 La1 C3 C2 79.9(3) . . . . ? N1 La1 C3 C2 -1.6(3) . . . . ? N2 La1 C3 C2 163.2(3) . . . . ? C20 La1 C3 C2 -120.0(3) . . . . ? C21 La1 C3 C2 -90.4(3) . . . . ? C4 La1 C3 C2 -112.0(4) . . . . ? C19 La1 C3 C2 -148.7(3) . . . . ? C1 La1 C3 C2 -36.3(3) . . . . ? C9 La1 C3 C2 -75.2(3) . . . . ? C22 La1 C3 C2 -84.6(4) . . . . ? N3 La1 C3 C4 -168.1(3) . . . . ? N1 La1 C3 C4 110.4(3) . . . . ? N2 La1 C3 C4 -84.8(3) . . . . ? C20 La1 C3 C4 -8.0(3) . . . . ? C21 La1 C3 C4 21.6(3) . . . . ? C2 La1 C3 C4 112.0(4) . . . . ? C19 La1 C3 C4 -36.7(3) . . . . ? C1 La1 C3 C4 75.7(3) . . . . ? C9 La1 C3 C4 36.8(3) . . . . ? C22 La1 C3 C4 27.4(5) . . . . ? C2 C3 C4 C5 -173.5(5) . . . . ? La1 C3 C4 C5 114.3(5) . . . . ? C2 C3 C4 C9 1.9(5) . . . . ? La1 C3 C4 C9 -70.3(3) . . . . ? C2 C3 C4 La1 72.2(3) . . . . ? N3 La1 C4 C3 14.1(3) . . . . ? N1 La1 C4 C3 -81.9(3) . . . . ? N2 La1 C4 C3 86.2(3) . . . . ? C20 La1 C4 C3 172.6(3) . . . . ? C21 La1 C4 C3 -162.0(3) . . . . ? C2 La1 C4 C3 -37.6(3) . . . . ? C19 La1 C4 C3 150.5(3) . . . . ? C1 La1 C4 C3 -76.7(3) . . . . ? C9 La1 C4 C3 -113.3(4) . . . . ? C22 La1 C4 C3 -164.4(3) . . . . ? N3 La1 C4 C5 -115.2(4) . . . . ? N1 La1 C4 C5 148.7(4) . . . . ? N2 La1 C4 C5 -43.2(4) . . . . ? C3 La1 C4 C5 -129.3(5) . . . . ? C20 La1 C4 C5 43.2(4) . . . . ? C21 La1 C4 C5 68.7(4) . . . . ? C2 La1 C4 C5 -166.9(5) . . . . ? C19 La1 C4 C5 21.2(4) . . . . ? C1 La1 C4 C5 153.9(5) . . . . ? C9 La1 C4 C5 117.3(5) . . . . ? C22 La1 C4 C5 66.2(4) . . . . ? N3 La1 C4 C9 127.5(3) . . . . ? N1 La1 C4 C9 31.4(3) . . . . ? N2 La1 C4 C9 -160.5(3) . . . . ? C3 La1 C4 C9 113.3(4) . . . . ? C20 La1 C4 C9 -74.1(3) . . . . ? C21 La1 C4 C9 -48.7(3) . . . . ? C2 La1 C4 C9 75.8(3) . . . . ? C19 La1 C4 C9 -96.2(3) . . . . ? C1 La1 C4 C9 36.6(2) . . . . ? C22 La1 C4 C9 -51.1(3) . . . . ? C3 C4 C5 C6 174.4(5) . . . . ? C9 C4 C5 C6 -0.6(7) . . . . ? La1 C4 C5 C6 -92.7(5) . . . . ? C4 C5 C6 C7 0.6(8) . . . . ? C5 C6 C7 C8 0.9(8) . . . . ? C6 C7 C8 C9 -2.4(7) . . . . ? C7 C8 C9 C1 -171.9(5) . . . . ? C7 C8 C9 C4 2.4(6) . . . . ? C7 C8 C9 La1 89.6(5) . . . . ? C2 C1 C9 C8 174.9(5) . . . . ? C10 C1 C9 C8 3.0(8) . . . . ? La1 C1 C9 C8 -117.7(5) . . . . ? C2 C1 C9 C4 0.3(5) . . . . ? C10 C1 C9 C4 -171.7(4) . . . . ? La1 C1 C9 C4 67.6(3) . . . . ? C2 C1 C9 La1 -67.4(3) . . . . ? C10 C1 C9 La1 120.7(5) . . . . ? C3 C4 C9 C8 -177.0(4) . . . . ? C5 C4 C9 C8 -0.9(6) . . . . ? La1 C4 C9 C8 116.0(4) . . . . ? C3 C4 C9 C1 -1.3(5) . . . . ? C5 C4 C9 C1 174.8(4) . . . . ? La1 C4 C9 C1 -68.3(3) . . . . ? C3 C4 C9 La1 67.0(3) . . . . ? C5 C4 C9 La1 -116.9(4) . . . . ? N3 La1 C9 C8 172.3(4) . . . . ? N1 La1 C9 C8 93.8(4) . . . . ? N2 La1 C9 C8 -95.1(4) . . . . ? C3 La1 C9 C8 -150.6(5) . . . . ? C20 La1 C9 C8 -12.5(4) . . . . ? C21 La1 C9 C8 16.6(4) . . . . ? C2 La1 C9 C8 169.8(5) . . . . ? C4 La1 C9 C8 -113.9(5) . . . . ? C19 La1 C9 C8 -23.2(4) . . . . ? C1 La1 C9 C8 133.0(5) . . . . ? C22 La1 C9 C8 24.8(4) . . . . ? N3 La1 C9 C1 39.4(4) . . . . ? N1 La1 C9 C1 -39.2(3) . . . . ? N2 La1 C9 C1 132.0(3) . . . . ? C3 La1 C9 C1 76.5(3) . . . . ? C20 La1 C9 C1 -145.4(3) . . . . ? C21 La1 C9 C1 -116.4(3) . . . . ? C2 La1 C9 C1 36.9(3) . . . . ? C4 La1 C9 C1 113.2(4) . . . . ? C19 La1 C9 C1 -156.2(3) . . . . ? C22 La1 C9 C1 -108.2(3) . . . . ? N3 La1 C9 C4 -73.8(3) . . . . ? N1 La1 C9 C4 -152.4(3) . . . . ? N2 La1 C9 C4 18.8(3) . . . . ? C3 La1 C9 C4 -36.7(3) . . . . ? C20 La1 C9 C4 101.4(3) . . . . ? C21 La1 C9 C4 130.4(3) . . . . ? C2 La1 C9 C4 -76.3(3) . . . . ? C19 La1 C9 C4 90.6(3) . . . . ? C1 La1 C9 C4 -113.2(4) . . . . ? C22 La1 C9 C4 138.7(3) . . . . ? C2 C1 C10 C11 120.8(5) . . . . ? C9 C1 C10 C11 -68.6(6) . . . . ? La1 C1 C10 C11 29.4(6) . . . . ? C2 C1 C10 C17 -2.2(7) . . . . ? C9 C1 C10 C17 168.4(5) . . . . ? La1 C1 C10 C17 -93.6(4) . . . . ? C2 C1 C10 C18 -120.1(5) . . . . ? C9 C1 C10 C18 50.5(6) . . . . ? La1 C1 C10 C18 148.5(4) . . . . ? C1 C10 C11 C12 -83.0(6) . . . . ? C17 C10 C11 C12 40.6(6) . . . . ? C18 C10 C11 C12 159.0(5) . . . . ? C16 N1 C12 C13 -0.2(7) . . . . ? La1 N1 C12 C13 -176.0(4) . . . . ? C16 N1 C12 C11 179.9(5) . . . . ? La1 N1 C12 C11 4.1(7) . . . . ? C10 C11 C12 N1 66.9(6) . . . . ? C10 C11 C12 C13 -113.0(6) . . . . ? N1 C12 C13 C14 -0.4(9) . . . . ? C11 C12 C13 C14 179.6(6) . . . . ? C12 C13 C14 C15 1.1(11) . . . . ? C13 C14 C15 C16 -1.3(10) . . . . ? C12 N1 C16 C15 0.0(8) . . . . ? La1 N1 C16 C15 176.5(4) . . . . ? C14 C15 C16 N1 0.8(9) . . . . ? N3 La1 C19 C20 -169.8(3) . . . . ? N1 La1 C19 C20 -77.1(3) . . . . ? N2 La1 C19 C20 117.5(3) . . . . ? C3 La1 C19 C20 68.5(3) . . . . ? C21 La1 C19 C20 -36.4(3) . . . . ? C2 La1 C19 C20 40.5(4) . . . . ? C4 La1 C19 C20 51.6(3) . . . . ? C1 La1 C19 C20 8.3(3) . . . . ? C9 La1 C19 C20 22.4(3) . . . . ? C22 La1 C19 C20 -75.1(3) . . . . ? N3 La1 C19 C27 -58.4(3) . . . . ? N1 La1 C19 C27 34.3(3) . . . . ? N2 La1 C19 C27 -131.1(3) . . . . ? C3 La1 C19 C27 179.9(2) . . . . ? C20 La1 C19 C27 111.4(4) . . . . ? C21 La1 C19 C27 75.0(3) . . . . ? C2 La1 C19 C27 151.9(3) . . . . ? C4 La1 C19 C27 163.0(3) . . . . ? C1 La1 C19 C27 119.7(3) . . . . ? C9 La1 C19 C27 133.9(3) . . . . ? C22 La1 C19 C27 36.3(2) . . . . ? N3 La1 C19 C28 73.2(4) . . . . ? N1 La1 C19 C28 165.9(4) . . . . ? N2 La1 C19 C28 0.6(4) . . . . ? C3 La1 C19 C28 -48.5(4) . . . . ? C20 La1 C19 C28 -117.0(5) . . . . ? C21 La1 C19 C28 -153.3(4) . . . . ? C2 La1 C19 C28 -76.4(5) . . . . ? C4 La1 C19 C28 -65.3(4) . . . . ? C1 La1 C19 C28 -108.7(4) . . . . ? C9 La1 C19 C28 -94.5(4) . . . . ? C22 La1 C19 C28 167.9(4) . . . . ? C27 C19 C20 C21 -2.4(5) . . . . ? C28 C19 C20 C21 -169.6(4) . . . . ? La1 C19 C20 C21 70.6(3) . . . . ? C27 C19 C20 La1 -73.0(3) . . . . ? C28 C19 C20 La1 119.9(4) . . . . ? N3 La1 C20 C21 -97.6(4) . . . . ? N1 La1 C20 C21 -0.4(3) . . . . ? N2 La1 C20 C21 -170.9(3) . . . . ? C3 La1 C20 C21 120.2(3) . . . . ? C2 La1 C20 C21 90.4(3) . . . . ? C4 La1 C20 C21 116.4(3) . . . . ? C19 La1 C20 C21 -113.9(4) . . . . ? C1 La1 C20 C21 72.6(3) . . . . ? C9 La1 C20 C21 88.4(3) . . . . ? C22 La1 C20 C21 -37.2(2) . . . . ? N3 La1 C20 C19 16.3(4) . . . . ? N1 La1 C20 C19 113.5(3) . . . . ? N2 La1 C20 C19 -57.0(3) . . . . ? C3 La1 C20 C19 -125.9(3) . . . . ? C21 La1 C20 C19 113.9(4) . . . . ? C2 La1 C20 C19 -155.7(3) . . . . ? C4 La1 C20 C19 -129.7(3) . . . . ? C1 La1 C20 C19 -173.5(3) . . . . ? C9 La1 C20 C19 -157.7(3) . . . . ? C22 La1 C20 C19 76.7(3) . . . . ? C19 C20 C21 C22 3.2(5) . . . . ? La1 C20 C21 C22 75.6(3) . . . . ? C19 C20 C21 La1 -72.5(3) . . . . ? N3 La1 C21 C20 121.1(3) . . . . ? N1 La1 C21 C20 179.6(3) . . . . ? N2 La1 C21 C20 9.9(3) . . . . ? C3 La1 C21 C20 -74.1(3) . . . . ? C2 La1 C21 C20 -107.3(3) . . . . ? C4 La1 C21 C20 -63.9(3) . . . . ? C19 La1 C21 C20 36.6(2) . . . . ? C1 La1 C21 C20 -110.3(3) . . . . ? C9 La1 C21 C20 -85.3(3) . . . . ? C22 La1 C21 C20 111.8(4) . . . . ? N3 La1 C21 C22 9.3(4) . . . . ? N1 La1 C21 C22 67.8(3) . . . . ? N2 La1 C21 C22 -101.9(3) . . . . ? C3 La1 C21 C22 174.1(2) . . . . ? C20 La1 C21 C22 -111.8(4) . . . . ? C2 La1 C21 C22 140.9(3) . . . . ? C4 La1 C21 C22 -175.7(3) . . . . ? C19 La1 C21 C22 -75.2(3) . . . . ? C1 La1 C21 C22 137.9(3) . . . . ? C9 La1 C21 C22 162.8(3) . . . . ? C20 C21 C22 C23 174.7(5) . . . . ? La1 C21 C22 C23 -113.7(5) . . . . ? C20 C21 C22 C27 -2.6(5) . . . . ? La1 C21 C22 C27 69.0(3) . . . . ? C20 C21 C22 La1 -71.6(3) . . . . ? N3 La1 C22 C23 -45.0(4) . . . . ? N1 La1 C22 C23 24.3(4) . . . . ? N2 La1 C22 C23 -140.6(4) . . . . ? C3 La1 C22 C23 118.2(4) . . . . ? C20 La1 C22 C23 166.3(5) . . . . ? C21 La1 C22 C23 128.5(5) . . . . ? C2 La1 C22 C23 72.3(5) . . . . ? C4 La1 C22 C23 133.6(4) . . . . ? C19 La1 C22 C23 -153.8(5) . . . . ? C1 La1 C22 C23 82.4(4) . . . . ? C9 La1 C22 C23 111.1(4) . . . . ? N3 La1 C22 C21 -173.5(3) . . . . ? N1 La1 C22 C21 -104.2(3) . . . . ? N2 La1 C22 C21 90.9(3) . . . . ? C3 La1 C22 C21 -10.3(4) . . . . ? C20 La1 C22 C21 37.8(3) . . . . ? C2 La1 C22 C21 -56.2(3) . . . . ? C4 La1 C22 C21 5.1(3) . . . . ? C19 La1 C22 C21 77.7(3) . . . . ? C1 La1 C22 C21 -46.1(3) . . . . ? C9 La1 C22 C21 -17.4(3) . . . . ? N3 La1 C22 C27 73.1(3) . . . . ? N1 La1 C22 C27 142.4(3) . . . . ? N2 La1 C22 C27 -22.5(3) . . . . ? C3 La1 C22 C27 -123.7(3) . . . . ? C20 La1 C22 C27 -75.6(3) . . . . ? C21 La1 C22 C27 -113.4(4) . . . . ? C2 La1 C22 C27 -169.6(3) . . . . ? C4 La1 C22 C27 -108.3(3) . . . . ? C19 La1 C22 C27 -35.7(2) . . . . ? C1 La1 C22 C27 -159.5(2) . . . . ? C9 La1 C22 C27 -130.8(2) . . . . ? C21 C22 C23 C24 -175.8(5) . . . . ? C27 C22 C23 C24 1.1(7) . . . . ? La1 C22 C23 C24 93.5(5) . . . . ? C22 C23 C24 C25 -1.2(8) . . . . ? C23 C24 C25 C26 0.1(9) . . . . ? C24 C25 C26 C27 1.0(8) . . . . ? C20 C19 C27 C26 -174.6(5) . . . . ? C28 C19 C27 C26 -8.9(9) . . . . ? La1 C19 C27 C26 117.3(6) . . . . ? C20 C19 C27 C22 0.8(5) . . . . ? C28 C19 C27 C22 166.5(4) . . . . ? La1 C19 C27 C22 -67.3(3) . . . . ? C20 C19 C27 La1 68.1(3) . . . . ? C28 C19 C27 La1 -126.2(5) . . . . ? C25 C26 C27 C19 174.2(5) . . . . ? C25 C26 C27 C22 -0.9(7) . . . . ? C25 C26 C27 La1 -88.6(6) . . . . ? C23 C22 C27 C19 -176.5(4) . . . . ? C21 C22 C27 C19 1.1(5) . . . . ? La1 C22 C27 C19 65.8(3) . . . . ? C23 C22 C27 C26 -0.1(6) . . . . ? C21 C22 C27 C26 177.5(4) . . . . ? La1 C22 C27 C26 -117.7(4) . . . . ? C23 C22 C27 La1 117.6(4) . . . . ? C21 C22 C27 La1 -64.7(3) . . . . ? N3 La1 C27 C19 130.1(3) . . . . ? N1 La1 C27 C19 -149.4(3) . . . . ? N2 La1 C27 C19 45.2(3) . . . . ? C3 La1 C27 C19 -0.2(5) . . . . ? C20 La1 C27 C19 -38.3(2) . . . . ? C21 La1 C27 C19 -78.1(3) . . . . ? C2 La1 C27 C19 -86.1(6) . . . . ? C4 La1 C27 C19 -21.4(3) . . . . ? C1 La1 C27 C19 -85.9(3) . . . . ? C9 La1 C27 C19 -55.4(3) . . . . ? C22 La1 C27 C19 -114.6(4) . . . . ? N3 La1 C27 C26 -3.5(4) . . . . ? N1 La1 C27 C26 77.0(4) . . . . ? N2 La1 C27 C26 -88.3(4) . . . . ? C3 La1 C27 C26 -133.7(4) . . . . ? C20 La1 C27 C26 -171.9(4) . . . . ? C21 La1 C27 C26 148.3(4) . . . . ? C2 La1 C27 C26 140.4(6) . . . . ? C4 La1 C27 C26 -155.0(3) . . . . ? C19 La1 C27 C26 -133.5(5) . . . . ? C1 La1 C27 C26 140.5(4) . . . . ? C9 La1 C27 C26 171.1(3) . . . . ? C22 La1 C27 C26 111.8(5) . . . . ? N3 La1 C27 C22 -115.3(3) . . . . ? N1 La1 C27 C22 -34.8(3) . . . . ? N2 La1 C27 C22 159.8(3) . . . . ? C3 La1 C27 C22 114.4(3) . . . . ? C20 La1 C27 C22 76.3(3) . . . . ? C21 La1 C27 C22 36.5(3) . . . . ? C2 La1 C27 C22 28.5(7) . . . . ? C4 La1 C27 C22 93.2(3) . . . . ? C19 La1 C27 C22 114.6(4) . . . . ? C1 La1 C27 C22 28.7(3) . . . . ? C9 La1 C27 C22 59.3(3) . . . . ? C20 C19 C28 C36 68.1(6) . . . . ? C27 C19 C28 C36 -95.8(6) . . . . ? La1 C19 C28 C36 157.8(4) . . . . ? C20 C19 C28 C35 -172.6(4) . . . . ? C27 C19 C28 C35 23.5(7) . . . . ? La1 C19 C28 C35 -82.9(5) . . . . ? C20 C19 C28 C29 -49.2(6) . . . . ? C27 C19 C28 C29 146.9(5) . . . . ? La1 C19 C28 C29 40.4(6) . . . . ? C36 C28 C29 C30 160.9(5) . . . . ? C35 C28 C29 C30 44.2(7) . . . . ? C19 C28 C29 C30 -82.0(6) . . . . ? C34 N2 C30 C31 0.7(7) . . . . ? La1 N2 C30 C31 -173.7(4) . . . . ? C34 N2 C30 C29 -179.8(5) . . . . ? La1 N2 C30 C29 5.8(7) . . . . ? C28 C29 C30 N2 58.9(8) . . . . ? C28 C29 C30 C31 -121.6(6) . . . . ? N2 C30 C31 C32 1.2(10) . . . . ? C29 C30 C31 C32 -178.2(6) . . . . ? C30 C31 C32 C33 -2.2(12) . . . . ? C31 C32 C33 C34 1.1(11) . . . . ? C30 N2 C34 C33 -1.9(8) . . . . ? La1 N2 C34 C33 173.8(5) . . . . ? C32 C33 C34 N2 0.9(10) . . . . ? C41 C42 C43 C44 -174(3) . . . . ? C42 C43 C44 C45 23(11) . . . . ? C43 C44 C45 C46 -163(8) . . . . ? C41' C42' C43' C44' 159(4) . . . . ? C42' C43' C44' C45' -137(3) . . . . ? C43' C44' C45' C46' 168(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.704 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.057 #######################################