# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_mo_dm11526_0m _database_code_depnum_ccdc_archive 'CCDC 873791' #TrackingRef 'mo_dm11526_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H62 La N3 O2 Si2' _chemical_formula_weight 860.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 10.2282(8) _cell_length_b 20.2161(15) _cell_length_c 21.3805(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4420.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 9925 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 33.25 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 1.058 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7085 _exptl_absorpt_correction_T_max 0.8325 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42577 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 30.00 _reflns_number_total 12900 _reflns_number_gt 12261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+1.8416P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.452(7) _chemical_absolute_configuration ad _refine_ls_number_reflns 12900 _refine_ls_number_parameters 483 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 La1 La 0.843906(10) -0.014374(6) 0.129693(5) 0.01895(3) Uani 1 1 d . . . Si1 Si 0.74232(6) -0.17496(3) 0.08080(3) 0.02608(12) Uani 1 1 d . . . Si2 Si 0.95760(6) -0.17124(3) 0.17880(3) 0.02334(11) Uani 1 1 d . . . N1 N 1.06472(16) 0.05025(8) 0.11640(7) 0.0183(3) Uani 1 1 d . . . N2 N 0.62180(15) 0.05104(8) 0.13744(8) 0.0183(3) Uani 1 1 d . . . N3 N 0.84766(17) -0.13395(8) 0.12967(8) 0.0224(3) Uani 1 1 d . . . O1 O 0.89250(15) 0.04095(9) 0.21890(7) 0.0267(3) Uani 1 1 d . . . O2 O 0.79798(15) 0.03445(9) 0.03707(7) 0.0273(3) Uani 1 1 d . . . C1 C 0.9904(2) 0.06263(10) 0.25265(9) 0.0204(4) Uani 1 1 d . . . C2 C 0.9735(3) 0.07355(12) 0.31746(10) 0.0282(4) Uani 1 1 d . . . H2 H 0.8901 0.0667 0.3360 0.034 Uiso 1 1 calc R . . C3 C 1.0768(3) 0.09398(13) 0.35408(11) 0.0331(5) Uani 1 1 d . . . H3 H 1.0639 0.1005 0.3976 0.040 Uiso 1 1 calc R . . C4 C 1.2000(3) 0.10518(13) 0.32832(11) 0.0313(5) Uani 1 1 d . . . H4 H 1.2710 0.1180 0.3543 0.038 Uiso 1 1 calc R . . C5 C 1.2177(2) 0.09756(11) 0.26507(10) 0.0244(4) Uani 1 1 d . . . H5 H 1.3009 0.1068 0.2473 0.029 Uiso 1 1 calc R . . C6 C 1.1147(2) 0.07632(10) 0.22598(10) 0.0194(4) Uani 1 1 d . . . C7 C 1.13933(18) 0.07466(10) 0.15957(9) 0.0189(4) Uani 1 1 d . . . H7 H 1.2194 0.0936 0.1460 0.023 Uiso 1 1 calc R . . C8 C 1.09905(19) 0.06535(11) 0.05241(9) 0.0192(4) Uani 1 1 d . . . C9 C 1.13758(18) 0.01374(12) 0.01259(9) 0.0217(4) Uani 1 1 d . . . C10 C 1.1629(2) 0.02854(11) -0.05026(9) 0.0273(4) Uani 1 1 d . . . H10 H 1.1897 -0.0057 -0.0779 0.033 Uiso 1 1 calc R . . C11 C 1.1493(3) 0.09238(13) -0.07266(10) 0.0305(5) Uani 1 1 d . . . H11 H 1.1675 0.1018 -0.1153 0.037 Uiso 1 1 calc R . . C12 C 1.1092(2) 0.14244(13) -0.03294(11) 0.0294(5) Uani 1 1 d . . . H12 H 1.1002 0.1861 -0.0489 0.035 Uiso 1 1 calc R . . C13 C 1.0815(2) 0.13042(11) 0.03000(10) 0.0243(4) Uani 1 1 d . . . C14 C 1.0277(3) 0.18636(12) 0.06978(11) 0.0311(5) Uani 1 1 d . . . H14 H 1.0022 0.1675 0.1113 0.037 Uiso 1 1 calc R . . C15 C 0.9046(3) 0.21621(15) 0.03959(15) 0.0425(6) Uani 1 1 d . . . H15A H 0.9272 0.2352 -0.0012 0.064 Uiso 1 1 calc R . . H15B H 0.8694 0.2509 0.0668 0.064 Uiso 1 1 calc R . . H15C H 0.8388 0.1815 0.0339 0.064 Uiso 1 1 calc R . . C16 C 1.1308(3) 0.23943(15) 0.08119(15) 0.0480(7) Uani 1 1 d . . . H16A H 1.2070 0.2196 0.1017 0.072 Uiso 1 1 calc R . . H16B H 1.0943 0.2741 0.1081 0.072 Uiso 1 1 calc R . . H16C H 1.1573 0.2588 0.0411 0.072 Uiso 1 1 calc R . . C17 C 1.1559(2) -0.05638(10) 0.03647(9) 0.0235(4) Uani 1 1 d . . . H17 H 1.1141 -0.0593 0.0787 0.028 Uiso 1 1 calc R . . C18 C 1.3018(3) -0.07164(14) 0.04431(14) 0.0385(6) Uani 1 1 d . . . H18A H 1.3452 -0.0693 0.0035 0.058 Uiso 1 1 calc R . . H18B H 1.3124 -0.1162 0.0617 0.058 Uiso 1 1 calc R . . H18C H 1.3412 -0.0392 0.0727 0.058 Uiso 1 1 calc R . . C19 C 1.0894(3) -0.10714(13) -0.00600(12) 0.0340(5) Uani 1 1 d . . . H19A H 0.9981 -0.0943 -0.0127 0.051 Uiso 1 1 calc R . . H19B H 1.0926 -0.1508 0.0138 0.051 Uiso 1 1 calc R . . H19C H 1.1349 -0.1088 -0.0463 0.051 Uiso 1 1 calc R . . C20 C 0.7010(2) 0.05300(11) 0.00127(10) 0.0215(4) Uani 1 1 d . . . C21 C 0.7182(2) 0.05658(13) -0.06421(11) 0.0308(5) Uani 1 1 d . . . H21 H 0.8012 0.0466 -0.0818 0.037 Uiso 1 1 calc R . . C22 C 0.6169(3) 0.07419(14) -0.10287(11) 0.0343(5) Uani 1 1 d . . . H22 H 0.6307 0.0752 -0.1468 0.041 Uiso 1 1 calc R . . C23 C 0.4943(3) 0.09063(13) -0.07899(11) 0.0329(5) Uani 1 1 d . . . H23 H 0.4247 0.1021 -0.1063 0.039 Uiso 1 1 calc R . . C24 C 0.4757(2) 0.08995(11) -0.01506(10) 0.0257(4) Uani 1 1 d . . . H24 H 0.3933 0.1027 0.0016 0.031 Uiso 1 1 calc R . . C25 C 0.5768(2) 0.07071(10) 0.02613(10) 0.0198(4) Uani 1 1 d . . . C26 C 0.54986(19) 0.07342(10) 0.09243(9) 0.0200(4) Uani 1 1 d . . . H26 H 0.4702 0.0940 0.1043 0.024 Uiso 1 1 calc R . . C27 C 0.58863(19) 0.06931(11) 0.20065(9) 0.0200(4) Uani 1 1 d . . . C28 C 0.6000(2) 0.13547(12) 0.21983(10) 0.0252(4) Uani 1 1 d . . . C29 C 0.5836(2) 0.14948(13) 0.28369(11) 0.0309(5) Uani 1 1 d . . . H29 H 0.5909 0.1939 0.2978 0.037 Uiso 1 1 calc R . . C30 C 0.5570(3) 0.09994(14) 0.32649(11) 0.0333(5) Uani 1 1 d . . . H30 H 0.5475 0.1103 0.3696 0.040 Uiso 1 1 calc R . . C31 C 0.5444(2) 0.03548(13) 0.30646(10) 0.0307(5) Uani 1 1 d . . . H31 H 0.5242 0.0018 0.3360 0.037 Uiso 1 1 calc R . . C32 C 0.56077(19) 0.01869(13) 0.24346(9) 0.0244(4) Uani 1 1 d . . . C33 C 0.5434(2) -0.05263(12) 0.22315(11) 0.0262(4) Uani 1 1 d . . . H33 H 0.5784 -0.0568 0.1797 0.031 Uiso 1 1 calc R . . C34 C 0.3981(3) -0.07064(16) 0.22137(15) 0.0428(6) Uani 1 1 d . . . H34A H 0.3606 -0.0657 0.2633 0.064 Uiso 1 1 calc R . . H34B H 0.3882 -0.1166 0.2075 0.064 Uiso 1 1 calc R . . H34C H 0.3526 -0.0412 0.1922 0.064 Uiso 1 1 calc R . . C35 C 0.6194(3) -0.10060(14) 0.26461(14) 0.0427(7) Uani 1 1 d . . . H35A H 0.7109 -0.0864 0.2673 0.064 Uiso 1 1 calc R . . H35B H 0.6152 -0.1451 0.2466 0.064 Uiso 1 1 calc R . . H35C H 0.5809 -0.1011 0.3066 0.064 Uiso 1 1 calc R . . C36 C 0.6282(3) 0.19281(13) 0.17571(12) 0.0361(6) Uani 1 1 d . . . H36 H 0.6520 0.1741 0.1340 0.043 Uiso 1 1 calc R . . C37 C 0.5052(5) 0.23447(17) 0.16776(17) 0.0637(11) Uani 1 1 d . . . H37A H 0.4349 0.2069 0.1506 0.096 Uiso 1 1 calc R . . H37B H 0.5232 0.2711 0.1390 0.096 Uiso 1 1 calc R . . H37C H 0.4784 0.2521 0.2085 0.096 Uiso 1 1 calc R . . C38 C 0.7428(5) 0.2346(2) 0.19877(17) 0.0737(14) Uani 1 1 d . . . H38A H 0.7178 0.2575 0.2374 0.111 Uiso 1 1 calc R . . H38B H 0.7659 0.2673 0.1668 0.111 Uiso 1 1 calc R . . H38C H 0.8181 0.2060 0.2069 0.111 Uiso 1 1 calc R . . C39 C 0.8207(3) -0.23850(14) 0.02885(14) 0.0415(6) Uani 1 1 d . . . H39A H 0.8969 -0.2190 0.0080 0.062 Uiso 1 1 calc R . . H39B H 0.7576 -0.2532 -0.0027 0.062 Uiso 1 1 calc R . . H39C H 0.8486 -0.2764 0.0541 0.062 Uiso 1 1 calc R . . C40 C 0.6599(3) -0.11383(14) 0.02739(14) 0.0417(6) Uani 1 1 d . . . H40A H 0.6181 -0.0792 0.0524 0.063 Uiso 1 1 calc R . . H40B H 0.5935 -0.1366 0.0023 0.063 Uiso 1 1 calc R . . H40C H 0.7251 -0.0939 -0.0004 0.063 Uiso 1 1 calc R . . C41 C 0.6064(3) -0.21962(14) 0.12262(15) 0.0408(6) Uani 1 1 d . . . H41A H 0.6438 -0.2513 0.1524 0.061 Uiso 1 1 calc R . . H41B H 0.5525 -0.2433 0.0921 0.061 Uiso 1 1 calc R . . H41C H 0.5523 -0.1875 0.1452 0.061 Uiso 1 1 calc R . . C42 C 0.8836(3) -0.22734(14) 0.23905(13) 0.0381(6) Uani 1 1 d . . . H42A H 0.8201 -0.2025 0.2641 0.057 Uiso 1 1 calc R . . H42B H 0.9526 -0.2446 0.2664 0.057 Uiso 1 1 calc R . . H42C H 0.8394 -0.2643 0.2182 0.057 Uiso 1 1 calc R . . C43 C 1.0873(3) -0.22070(14) 0.13808(13) 0.0401(6) Uani 1 1 d . . . H43A H 1.0462 -0.2516 0.1087 0.060 Uiso 1 1 calc R . . H43B H 1.1379 -0.2456 0.1691 0.060 Uiso 1 1 calc R . . H43C H 1.1456 -0.1908 0.1152 0.060 Uiso 1 1 calc R . . C44 C 1.0462(2) -0.10504(13) 0.22402(12) 0.0311(5) Uani 1 1 d . . . H44A H 1.0911 -0.0754 0.1948 0.047 Uiso 1 1 calc R . . H44B H 1.1105 -0.1256 0.2519 0.047 Uiso 1 1 calc R . . H44C H 0.9832 -0.0797 0.2489 0.047 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 La1 0.01624(4) 0.02128(5) 0.01933(5) -0.00115(4) -0.00188(4) -0.00115(4) Si1 0.0257(3) 0.0241(3) 0.0285(3) -0.0038(2) -0.0036(2) -0.0047(2) Si2 0.0243(3) 0.0227(3) 0.0230(3) 0.0010(2) -0.0008(2) 0.0008(2) N1 0.0176(7) 0.0215(8) 0.0157(8) -0.0009(6) 0.0010(6) 0.0011(6) N2 0.0175(7) 0.0223(7) 0.0151(8) -0.0014(6) 0.0015(6) -0.0027(5) N3 0.0220(7) 0.0217(7) 0.0235(7) -0.0005(6) -0.0015(9) -0.0020(6) O1 0.0187(6) 0.0407(9) 0.0207(7) -0.0064(6) 0.0009(6) -0.0043(6) O2 0.0194(7) 0.0436(10) 0.0189(7) 0.0018(6) 0.0007(6) 0.0015(6) C1 0.0234(9) 0.0211(9) 0.0168(9) -0.0031(7) -0.0001(7) 0.0014(7) C2 0.0354(11) 0.0329(11) 0.0162(9) -0.0021(8) 0.0038(9) 0.0004(10) C3 0.0470(14) 0.0361(12) 0.0161(10) -0.0036(8) -0.0029(9) 0.0018(10) C4 0.0376(12) 0.0339(12) 0.0225(11) -0.0031(9) -0.0116(9) -0.0004(10) C5 0.0241(10) 0.0265(10) 0.0226(10) -0.0012(8) -0.0068(8) -0.0011(8) C6 0.0215(9) 0.0204(9) 0.0164(9) -0.0009(7) -0.0024(7) 0.0010(7) C7 0.0155(8) 0.0223(8) 0.0190(9) -0.0018(7) 0.0004(7) 0.0006(7) C8 0.0147(8) 0.0267(10) 0.0161(9) -0.0013(7) 0.0005(7) -0.0008(7) C9 0.0194(8) 0.0293(9) 0.0164(8) -0.0024(8) -0.0001(7) -0.0020(9) C10 0.0272(9) 0.0382(12) 0.0164(8) -0.0027(7) 0.0009(8) -0.0001(9) C11 0.0315(11) 0.0444(13) 0.0156(9) 0.0046(8) 0.0003(10) -0.0005(11) C12 0.0315(11) 0.0340(12) 0.0227(11) 0.0080(9) 0.0000(9) 0.0025(9) C13 0.0231(9) 0.0290(11) 0.0209(10) 0.0025(8) 0.0000(8) 0.0029(8) C14 0.0395(12) 0.0278(11) 0.0260(11) 0.0032(8) 0.0040(10) 0.0081(10) C15 0.0413(15) 0.0368(14) 0.0494(17) 0.0032(12) 0.0045(13) 0.0110(12) C16 0.0536(19) 0.0409(15) 0.0494(17) -0.0113(13) -0.0115(14) 0.0029(13) C17 0.0268(9) 0.0269(9) 0.0169(8) -0.0036(7) 0.0020(9) -0.0005(9) C18 0.0330(12) 0.0367(13) 0.0457(15) 0.0033(12) -0.0058(11) 0.0027(10) C19 0.0407(14) 0.0336(13) 0.0276(12) -0.0082(10) -0.0005(10) -0.0062(11) C20 0.0220(9) 0.0253(10) 0.0172(9) 0.0013(7) -0.0006(7) -0.0039(8) C21 0.0318(11) 0.0417(13) 0.0188(10) 0.0000(9) 0.0057(9) -0.0002(10) C22 0.0420(13) 0.0451(14) 0.0157(10) 0.0038(9) -0.0013(9) -0.0057(11) C23 0.0353(13) 0.0402(13) 0.0231(11) 0.0071(10) -0.0096(9) -0.0020(10) C24 0.0235(10) 0.0303(11) 0.0233(10) 0.0024(8) -0.0048(8) -0.0019(8) C25 0.0213(9) 0.0216(9) 0.0165(9) -0.0003(7) -0.0018(7) -0.0031(7) C26 0.0181(8) 0.0230(9) 0.0190(9) -0.0009(7) 0.0007(7) -0.0017(7) C27 0.0156(8) 0.0302(10) 0.0143(9) -0.0010(8) 0.0008(7) 0.0011(7) C28 0.0232(10) 0.0330(11) 0.0195(10) -0.0043(8) 0.0026(8) -0.0015(8) C29 0.0316(12) 0.0391(13) 0.0220(11) -0.0095(9) 0.0030(9) 0.0005(10) C30 0.0340(12) 0.0491(15) 0.0169(10) -0.0042(10) 0.0020(9) 0.0038(11) C31 0.0288(11) 0.0448(13) 0.0185(10) 0.0052(9) 0.0039(8) 0.0050(9) C32 0.0186(8) 0.0352(11) 0.0193(9) 0.0020(9) 0.0025(7) 0.0028(9) C33 0.0246(10) 0.0306(11) 0.0233(10) 0.0071(8) 0.0036(8) -0.0001(9) C34 0.0263(12) 0.0522(17) 0.0499(17) -0.0047(14) 0.0015(12) -0.0076(12) C35 0.0511(17) 0.0369(14) 0.0400(15) 0.0099(12) -0.0068(12) 0.0066(12) C36 0.0515(16) 0.0319(12) 0.0248(11) -0.0055(9) 0.0112(10) -0.0101(11) C37 0.101(3) 0.0421(17) 0.0484(18) 0.0150(14) 0.022(2) 0.0192(19) C38 0.101(3) 0.077(3) 0.0435(18) -0.0185(18) 0.020(2) -0.061(3) C39 0.0445(16) 0.0351(13) 0.0449(15) -0.0168(11) 0.0021(12) -0.0061(11) C40 0.0393(13) 0.0394(13) 0.0463(15) 0.0020(11) -0.0195(14) -0.0061(13) C41 0.0343(12) 0.0425(14) 0.0456(16) -0.0055(13) 0.0016(12) -0.0148(10) C42 0.0421(14) 0.0344(13) 0.0377(14) 0.0113(11) -0.0006(11) -0.0028(11) C43 0.0428(14) 0.0436(14) 0.0338(14) 0.0012(11) 0.0014(12) 0.0188(11) C44 0.0293(11) 0.0335(12) 0.0305(12) 0.0017(10) -0.0066(10) -0.0022(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O2 2.2620(16) . ? La1 O1 2.2661(16) . ? La1 N3 2.4176(16) . ? La1 N1 2.6246(17) . ? La1 N2 2.6338(16) . ? La1 Si2 3.5372(6) . ? Si1 N3 1.7148(18) . ? Si1 C39 1.878(3) . ? Si1 C40 1.882(3) . ? Si1 C41 1.883(3) . ? Si2 N3 1.7135(18) . ? Si2 C43 1.876(3) . ? Si2 C42 1.876(3) . ? Si2 C44 1.884(3) . ? N1 C7 1.295(2) . ? N1 C8 1.445(3) . ? N2 C26 1.293(3) . ? N2 C27 1.442(3) . ? O1 C1 1.310(3) . ? O2 C20 1.308(3) . ? C1 C2 1.414(3) . ? C1 C6 1.421(3) . ? C2 C3 1.379(3) . ? C2 H2 0.9500 . ? C3 C4 1.393(4) . ? C3 H3 0.9500 . ? C4 C5 1.373(3) . ? C4 H4 0.9500 . ? C5 C6 1.412(3) . ? C5 H5 0.9500 . ? C6 C7 1.442(3) . ? C7 H7 0.9500 . ? C8 C9 1.403(3) . ? C8 C13 1.411(3) . ? C9 C10 1.401(3) . ? C9 C17 1.518(3) . ? C10 C11 1.384(3) . ? C10 H10 0.9500 . ? C11 C12 1.383(3) . ? C11 H11 0.9500 . ? C12 C13 1.396(3) . ? C12 H12 0.9500 . ? C13 C14 1.518(3) . ? C14 C16 1.524(4) . ? C14 C15 1.539(4) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.530(3) . ? C17 C18 1.533(4) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.413(3) . ? C20 C25 1.423(3) . ? C21 C22 1.372(4) . ? C21 H21 0.9500 . ? C22 C23 1.394(4) . ? C22 H22 0.9500 . ? C23 C24 1.380(3) . ? C23 H23 0.9500 . ? C24 C25 1.412(3) . ? C24 H24 0.9500 . ? C25 C26 1.445(3) . ? C26 H26 0.9500 . ? C27 C32 1.402(3) . ? C27 C28 1.404(3) . ? C28 C29 1.405(3) . ? C28 C36 1.522(3) . ? C29 C30 1.383(4) . ? C29 H29 0.9500 . ? C30 C31 1.378(4) . ? C30 H30 0.9500 . ? C31 C32 1.399(3) . ? C31 H31 0.9500 . ? C32 C33 1.516(3) . ? C33 C35 1.527(3) . ? C33 C34 1.530(3) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.524(5) . ? C36 C38 1.527(4) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La1 O1 124.54(7) . . ? O2 La1 N3 116.07(6) . . ? O1 La1 N3 119.35(6) . . ? O2 La1 N1 82.34(5) . . ? O1 La1 N1 69.93(5) . . ? N3 La1 N1 118.95(6) . . ? O2 La1 N2 69.93(5) . . ? O1 La1 N2 83.59(5) . . ? N3 La1 N2 121.05(5) . . ? N1 La1 N2 119.94(5) . . ? O2 La1 Si2 136.00(4) . . ? O1 La1 Si2 96.92(5) . . ? N3 La1 Si2 25.63(4) . . ? N1 La1 Si2 101.27(4) . . ? N2 La1 Si2 135.65(4) . . ? N3 Si1 C39 115.02(11) . . ? N3 Si1 C40 109.49(10) . . ? C39 Si1 C40 106.35(14) . . ? N3 Si1 C41 113.97(11) . . ? C39 Si1 C41 105.55(13) . . ? C40 Si1 C41 105.80(14) . . ? N3 Si2 C43 114.47(11) . . ? N3 Si2 C42 114.98(11) . . ? C43 Si2 C42 106.37(13) . . ? N3 Si2 C44 108.53(10) . . ? C43 Si2 C44 106.06(13) . . ? C42 Si2 C44 105.74(12) . . ? N3 Si2 La1 37.61(5) . . ? C43 Si2 La1 124.94(9) . . ? C42 Si2 La1 127.83(9) . . ? C44 Si2 La1 70.95(8) . . ? C7 N1 C8 116.81(17) . . ? C7 N1 La1 128.27(13) . . ? C8 N1 La1 114.63(12) . . ? C26 N2 C27 118.31(17) . . ? C26 N2 La1 128.29(13) . . ? C27 N2 La1 112.99(12) . . ? Si2 N3 Si1 124.97(10) . . ? Si2 N3 La1 116.76(8) . . ? Si1 N3 La1 118.27(9) . . ? C1 O1 La1 142.80(14) . . ? C20 O2 La1 142.67(14) . . ? O1 C1 C2 119.9(2) . . ? O1 C1 C6 121.88(18) . . ? C2 C1 C6 118.2(2) . . ? C3 C2 C1 120.6(2) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 121.2(2) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 119.4(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.2(2) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 119.33(19) . . ? C5 C6 C7 117.33(19) . . ? C1 C6 C7 123.16(18) . . ? N1 C7 C6 127.40(18) . . ? N1 C7 H7 116.3 . . ? C6 C7 H7 116.3 . . ? C9 C8 C13 121.51(19) . . ? C9 C8 N1 119.06(19) . . ? C13 C8 N1 119.17(18) . . ? C10 C9 C8 118.4(2) . . ? C10 C9 C17 119.95(19) . . ? C8 C9 C17 121.65(17) . . ? C11 C10 C9 120.8(2) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 C10 120.0(2) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 121.6(2) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C12 C13 C8 117.6(2) . . ? C12 C13 C14 118.9(2) . . ? C8 C13 C14 123.4(2) . . ? C13 C14 C16 111.3(2) . . ? C13 C14 C15 110.7(2) . . ? C16 C14 C15 110.9(2) . . ? C13 C14 H14 107.9 . . ? C16 C14 H14 107.9 . . ? C15 C14 H14 107.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C9 C17 C19 111.81(18) . . ? C9 C17 C18 110.2(2) . . ? C19 C17 C18 111.3(2) . . ? C9 C17 H17 107.8 . . ? C19 C17 H17 107.8 . . ? C18 C17 H17 107.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O2 C20 C21 120.0(2) . . ? O2 C20 C25 122.05(19) . . ? C21 C20 C25 117.9(2) . . ? C22 C21 C20 121.1(2) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 121.3(2) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C24 C23 C22 119.0(2) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C25 121.3(2) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C24 C25 C20 119.33(19) . . ? C24 C25 C26 117.50(19) . . ? C20 C25 C26 123.08(19) . . ? N2 C26 C25 127.48(19) . . ? N2 C26 H26 116.3 . . ? C25 C26 H26 116.3 . . ? C32 C27 C28 121.4(2) . . ? C32 C27 N2 118.21(19) . . ? C28 C27 N2 119.90(19) . . ? C27 C28 C29 117.8(2) . . ? C27 C28 C36 124.1(2) . . ? C29 C28 C36 118.1(2) . . ? C30 C29 C28 121.4(2) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C31 C30 C29 119.8(2) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 121.2(2) . . ? C30 C31 H31 119.4 . . ? C32 C31 H31 119.4 . . ? C31 C32 C27 118.4(2) . . ? C31 C32 C33 119.5(2) . . ? C27 C32 C33 122.06(19) . . ? C32 C33 C35 112.2(2) . . ? C32 C33 C34 110.3(2) . . ? C35 C33 C34 111.0(2) . . ? C32 C33 H33 107.7 . . ? C35 C33 H33 107.7 . . ? C34 C33 H33 107.7 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C28 C36 C37 109.5(2) . . ? C28 C36 C38 111.5(3) . . ? C37 C36 C38 111.3(3) . . ? C28 C36 H36 108.1 . . ? C37 C36 H36 108.1 . . ? C38 C36 H36 108.1 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si1 C39 H39A 109.5 . . ? Si1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si1 C40 H40A 109.5 . . ? Si1 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si1 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si1 C41 H41A 109.5 . . ? Si1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si2 C42 H42A 109.5 . . ? Si2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si2 C43 H43A 109.5 . . ? Si2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si2 C44 H44A 109.5 . . ? Si2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.631 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.052