Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'John Belot' 'Victor W. Day' 'Arnold Rheingold' 'Steven A. Schuetz' _publ_contact_author_name 'Prof John Belot' _publ_contact_author_address ; Department of Chemistry University of Nebraska 621 HaH Lincoln NE 68588-0304 UNITED STATES OF AMERICA ; _publ_contact_author_email JBELOT2@UNL.EDU _publ_section_title ; Solvent influence on the formation of mononuclear or multinuclear lanthanum complexes containing tetradentate Schiff-base ligands ; data_belo11 _database_code_CSD 212787 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tris[bis-5,5’-(1,3-propanediyldiimino)-2,2-dimethyl-4-hexene-3-onato] lanthanum dimer ; _chemical_name_common ? _chemical_melting_point 166-167.5 _chemical_formula_moiety ? _chemical_formula_sum 'C57 H96 La2 N6 O6' _chemical_formula_weight 1239.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8880(14) _cell_length_b 18.9160(17) _cell_length_c 20.4748(19) _cell_angle_alpha 90.00 _cell_angle_beta 92.124(2) _cell_angle_gamma 90.00 _cell_volume 6149.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2568 _exptl_absorpt_coefficient_mu 1.420 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.3963 _exptl_absorpt_correction_T_max 0.6753 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 SMART APEX CCD Area Detector' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 71093 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.33 _reflns_number_total 14797 _reflns_number_gt 13100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections except 2 which were flagged by the user for potential systematic errors. 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^)+(0.0368P)^2^+4.7885P] 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 14797 _refine_ls_number_parameters 664 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0782 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.140839(8) 0.158901(7) 0.235127(7) 0.04181(5) Uani 1 1 d . . . La2 La 0.351438(7) 0.046256(6) 0.252569(6) 0.03399(4) Uani 1 1 d . . . O1 O 0.01268(13) 0.16090(10) 0.28943(10) 0.0585(5) Uani 1 1 d . . . O2 O 0.05335(10) 0.13066(9) 0.14573(9) 0.0467(4) Uani 1 1 d . . . O21 O 0.47387(11) 0.04380(9) 0.19237(9) 0.0452(4) Uani 1 1 d . . . O22 O 0.23551(10) 0.09678(8) 0.32274(8) 0.0394(3) Uani 1 1 d . . . O41 O 0.33090(10) -0.05240(9) 0.31981(9) 0.0443(4) Uani 1 1 d . . . O42 O 0.28248(10) 0.14402(8) 0.18202(8) 0.0393(3) Uani 1 1 d . . . N1 N 0.13474(17) 0.26719(13) 0.30796(15) 0.0721(8) Uani 1 1 d . . . N2 N 0.11850(14) 0.27312(12) 0.16545(14) 0.0581(6) Uani 1 1 d . . . N21 N 0.34853(12) -0.06021(10) 0.16477(10) 0.0403(4) Uani 1 1 d . . . N22 N 0.17894(13) 0.01695(10) 0.21279(10) 0.0413(4) Uani 1 1 d . . . N41 N 0.47252(13) 0.03785(11) 0.34606(11) 0.0459(5) Uani 1 1 d . . . N42 N 0.39562(13) 0.17926(11) 0.29025(10) 0.0436(4) Uani 1 1 d . . . C1 C -0.1155(2) 0.1679(2) 0.34530(18) 0.0838(12) Uani 1 1 d . . . C2 C -0.0278(2) 0.19622(19) 0.33221(15) 0.0669(9) Uani 1 1 d . . . C3 C 0.0042(3) 0.2575(2) 0.36120(17) 0.0833(12) Uani 1 1 d . . . H3 H -0.0287 0.2786 0.3931 0.100 Uiso 1 1 calc R . . C4 C 0.0819(3) 0.29186(19) 0.34773(19) 0.0826(12) Uani 1 1 d . . . C5 C 0.2103(2) 0.31000(18) 0.2922(2) 0.0970(15) Uani 1 1 d . . . H5A H 0.2560 0.2781 0.2805 0.116 Uiso 1 1 calc R . . H5B H 0.2293 0.3365 0.3312 0.116 Uiso 1 1 calc R . . C6 C 0.1929(2) 0.36103(17) 0.2368(2) 0.0942(14) Uani 1 1 d . . . H6A H 0.1405 0.3864 0.2447 0.113 Uiso 1 1 calc R . . H6B H 0.2385 0.3960 0.2365 0.113 Uiso 1 1 calc R . . C7 C 0.1854(2) 0.32653(16) 0.1711(2) 0.0821(12) Uani 1 1 d . . . H7A H 0.1746 0.3631 0.1380 0.098 Uiso 1 1 calc R . . H7B H 0.2393 0.3041 0.1619 0.098 Uiso 1 1 calc R . . C8 C 0.04902(16) 0.28792(14) 0.13322(13) 0.0484(6) Uani 1 1 d . . . C9 C -0.01478(15) 0.23689(14) 0.11634(13) 0.0474(6) Uani 1 1 d . . . H9 H -0.0669 0.2554 0.1014 0.057 Uiso 1 1 calc R . . C10 C -0.00969(14) 0.16501(13) 0.11910(11) 0.0411(5) Uani 1 1 d . . . C11 C -0.07843(16) 0.11778(15) 0.08782(14) 0.0536(7) Uani 1 1 d . . . C12 C -0.1500(4) 0.1932(4) 0.4098(3) 0.156(3) Uani 1 1 d . . . H12A H -0.1126 0.1782 0.4457 0.235 Uiso 1 1 calc R . . H12B H -0.2055 0.1731 0.4153 0.235 Uiso 1 1 calc R . . H12C H -0.1539 0.2444 0.4096 0.235 Uiso 1 1 calc R . . C13 C -0.1155(2) 0.0875(3) 0.3430(2) 0.0971(14) Uani 1 1 d . . . H13A H -0.0816 0.0692 0.3796 0.146 Uiso 1 1 calc R . . H13B H -0.0921 0.0718 0.3024 0.146 Uiso 1 1 calc R . . H13C H -0.1727 0.0702 0.3456 0.146 Uiso 1 1 calc R . . C14 C -0.1748(3) 0.1954(3) 0.2898(3) 0.1138(17) Uani 1 1 d . . . H14A H -0.1538 0.1806 0.2480 0.171 Uiso 1 1 calc R . . H14B H -0.1771 0.2466 0.2915 0.171 Uiso 1 1 calc R . . H14C H -0.2308 0.1762 0.2948 0.171 Uiso 1 1 calc R . . C15 C 0.0966(3) 0.3606(2) 0.3862(2) 0.124(2) Uani 1 1 d . . . H15A H 0.1499 0.3578 0.4107 0.187 Uiso 1 1 calc R . . H15B H 0.0514 0.3674 0.4161 0.187 Uiso 1 1 calc R . . H15C H 0.0979 0.4001 0.3560 0.187 Uiso 1 1 calc R . . C16 C 0.0290(2) 0.36156(16) 0.10713(17) 0.0646(8) Uani 1 1 d . . . H16A H 0.0579 0.3965 0.1344 0.097 Uiso 1 1 calc R . . H16B H -0.0313 0.3696 0.1077 0.097 Uiso 1 1 calc R . . H16C H 0.0475 0.3655 0.0627 0.097 Uiso 1 1 calc R . . C17 C -0.15681(18) 0.15675(18) 0.06321(17) 0.0670(8) Uani 1 1 d . . . H17A H -0.1960 0.1234 0.0428 0.100 Uiso 1 1 calc R . . H17B H -0.1414 0.1921 0.0315 0.100 Uiso 1 1 calc R . . H17C H -0.1831 0.1797 0.0996 0.100 Uiso 1 1 calc R . . C18 C -0.1044(3) 0.0638(2) 0.1378(3) 0.119(2) Uani 1 1 d . . . H18A H -0.1408 0.0288 0.1167 0.179 Uiso 1 1 calc R . . H18B H -0.1345 0.0873 0.1720 0.179 Uiso 1 1 calc R . . H18C H -0.0547 0.0408 0.1567 0.179 Uiso 1 1 calc R . . C19 C -0.0405(3) 0.0793(4) 0.0313(3) 0.165(3) Uani 1 1 d . . . H19A H -0.0828 0.0489 0.0105 0.247 Uiso 1 1 calc R . . H19B H 0.0067 0.0509 0.0474 0.247 Uiso 1 1 calc R . . H19C H -0.0212 0.1134 -0.0002 0.247 Uiso 1 1 calc R . . C21 C 0.60594(18) 0.03426(15) 0.14091(16) 0.0558(7) Uani 1 1 d . . . C22 C 0.51419(16) 0.01017(12) 0.14847(12) 0.0431(5) Uani 1 1 d . . . C23 C 0.48093(17) -0.04477(13) 0.11239(13) 0.0469(6) Uani 1 1 d . . . H23 H 0.5134 -0.0617 0.0782 0.056 Uiso 1 1 calc R . . C24 C 0.40184(16) -0.07912(12) 0.12129(12) 0.0443(5) Uani 1 1 d . . . C25 C 0.27373(15) -0.10517(12) 0.17266(13) 0.0448(5) Uani 1 1 d . . . H25A H 0.2586 -0.1046 0.2186 0.054 Uiso 1 1 calc R . . H25B H 0.2877 -0.1540 0.1612 0.054 Uiso 1 1 calc R . . C26 C 0.19804(16) -0.08122(13) 0.13043(13) 0.0492(6) Uani 1 1 d . . . H26A H 0.1500 -0.1119 0.1389 0.059 Uiso 1 1 calc R . . H26B H 0.2111 -0.0864 0.0843 0.059 Uiso 1 1 calc R . . C27 C 0.17369(17) -0.00451(13) 0.14349(12) 0.0474(6) Uani 1 1 d . . . H27A H 0.2105 0.0264 0.1188 0.057 Uiso 1 1 calc R . . H27B H 0.1159 0.0031 0.1266 0.057 Uiso 1 1 calc R . . C28 C 0.12364(15) -0.00637(12) 0.25301(12) 0.0422(5) Uani 1 1 d . . . C29 C 0.12438(15) 0.01421(12) 0.32081(12) 0.0423(5) Uani 1 1 d . . . H29 H 0.0819 -0.0054 0.3459 0.051 Uiso 1 1 calc R . . C30 C 0.18003(14) 0.05928(12) 0.35325(12) 0.0383(5) Uani 1 1 d . . . C31 C 0.17928(15) 0.06941(13) 0.42752(12) 0.0441(5) Uani 1 1 d . . . C32 C 0.6490(2) 0.0002(2) 0.0847(2) 0.0962(14) Uani 1 1 d . . . H32A H 0.6169 0.0095 0.0444 0.144 Uiso 1 1 calc R . . H32B H 0.6524 -0.0505 0.0918 0.144 Uiso 1 1 calc R . . H32C H 0.7053 0.0194 0.0817 0.144 Uiso 1 1 calc R . . C33 C 0.6534(2) 0.0127(3) 0.2049(2) 0.0994(14) Uani 1 1 d . . . H33A H 0.7115 0.0282 0.2037 0.149 Uiso 1 1 calc R . . H33B H 0.6518 -0.0383 0.2096 0.149 Uiso 1 1 calc R . . H33C H 0.6268 0.0345 0.2417 0.149 Uiso 1 1 calc R . . C34 C 0.6090(3) 0.11325(18) 0.1351(3) 0.0996(15) Uani 1 1 d . . . H34A H 0.5802 0.1278 0.0948 0.149 Uiso 1 1 calc R . . H34B H 0.6673 0.1286 0.1350 0.149 Uiso 1 1 calc R . . H34C H 0.5817 0.1344 0.1719 0.149 Uiso 1 1 calc R . . C35 C 0.3872(2) -0.14278(14) 0.07647(15) 0.0591(7) Uani 1 1 d . . . H35A H 0.3325 -0.1387 0.0542 0.089 Uiso 1 1 calc R . . H35B H 0.3893 -0.1858 0.1023 0.089 Uiso 1 1 calc R . . H35C H 0.4307 -0.1443 0.0444 0.089 Uiso 1 1 calc R . . C36 C 0.05315(17) -0.05690(16) 0.23338(15) 0.0581(7) Uani 1 1 d . . . H36A H 0.0421 -0.0541 0.1865 0.087 Uiso 1 1 calc R . . H36B H 0.0027 -0.0442 0.2559 0.087 Uiso 1 1 calc R . . H36C H 0.0696 -0.1048 0.2451 0.087 Uiso 1 1 calc R . . C37 C 0.1710(2) 0.14826(15) 0.44239(15) 0.0587(7) Uani 1 1 d . . . H37A H 0.1155 0.1646 0.4278 0.088 Uiso 1 1 calc R . . H37B H 0.2136 0.1743 0.4197 0.088 Uiso 1 1 calc R . . H37C H 0.1785 0.1559 0.4891 0.088 Uiso 1 1 calc R . . C38 C 0.26412(18) 0.04272(18) 0.45668(14) 0.0592(7) Uani 1 1 d . . . H38A H 0.2672 0.0521 0.5033 0.089 Uiso 1 1 calc R . . H38B H 0.3098 0.0670 0.4359 0.089 Uiso 1 1 calc R . . H38C H 0.2688 -0.0077 0.4492 0.089 Uiso 1 1 calc R . . C39 C 0.10878(19) 0.02890(16) 0.46018(14) 0.0570(7) Uani 1 1 d . . . H39A H 0.0546 0.0458 0.4433 0.086 Uiso 1 1 calc R . . H39B H 0.1130 0.0364 0.5070 0.086 Uiso 1 1 calc R . . H39C H 0.1140 -0.0212 0.4509 0.086 Uiso 1 1 calc R . . C41 C 0.32168(16) -0.16139(13) 0.37828(15) 0.0506(6) Uani 1 1 d . . . C42 C 0.36645(15) -0.09119(13) 0.36450(12) 0.0426(5) Uani 1 1 d . . . C43 C 0.44086(16) -0.07415(15) 0.39610(14) 0.0537(6) Uani 1 1 d . . . H43 H 0.4611 -0.1065 0.4278 0.064 Uiso 1 1 calc R . . C44 C 0.49176(16) -0.01286(15) 0.38669(14) 0.0525(6) Uani 1 1 d . . . C45 C 0.53078(17) 0.09800(15) 0.34131(14) 0.0554(7) Uani 1 1 d . . . H45A H 0.5349 0.1114 0.2953 0.066 Uiso 1 1 calc R . . H45B H 0.5869 0.0835 0.3576 0.066 Uiso 1 1 calc R . . C46 C 0.5023(2) 0.16163(16) 0.38002(15) 0.0642(8) Uani 1 1 d . . . H46A H 0.5408 0.2011 0.3729 0.077 Uiso 1 1 calc R . . H46B H 0.5055 0.1500 0.4267 0.077 Uiso 1 1 calc R . . C47 C 0.41258(19) 0.18487(16) 0.36117(13) 0.0557(7) Uani 1 1 d . . . H47A H 0.3725 0.1553 0.3840 0.067 Uiso 1 1 calc R . . H47B H 0.4045 0.2339 0.3750 0.067 Uiso 1 1 calc R . . C48 C 0.41123(15) 0.23178(13) 0.25252(13) 0.0446(5) Uani 1 1 d . . . C49 C 0.39297(15) 0.22778(13) 0.18283(12) 0.0435(5) Uani 1 1 d . . . H49 H 0.4257 0.2568 0.1564 0.052 Uiso 1 1 calc R . . C50 C 0.33423(15) 0.18708(12) 0.15115(12) 0.0408(5) Uani 1 1 d . . . C51 C 0.32529(18) 0.18632(15) 0.07631(13) 0.0514(6) Uani 1 1 d . . . C52 C 0.3483(2) -0.19568(19) 0.44271(17) 0.0768(10) Uani 1 1 d . . . H52A H 0.3394 -0.1628 0.4782 0.115 Uiso 1 1 calc R . . H52B H 0.4075 -0.2082 0.4421 0.115 Uiso 1 1 calc R . . H52C H 0.3151 -0.2380 0.4490 0.115 Uiso 1 1 calc R . . C53 C 0.3437(2) -0.21169(16) 0.32228(18) 0.0695(9) Uani 1 1 d . . . H53A H 0.3109 -0.2547 0.3253 0.104 Uiso 1 1 calc R . . H53B H 0.4032 -0.2231 0.3256 0.104 Uiso 1 1 calc R . . H53C H 0.3308 -0.1889 0.2807 0.104 Uiso 1 1 calc R . . C54 C 0.22642(19) -0.14971(17) 0.3750(2) 0.0789(11) Uani 1 1 d . . . H54A H 0.2104 -0.1215 0.4121 0.118 Uiso 1 1 calc R . . H54B H 0.1979 -0.1950 0.3760 0.118 Uiso 1 1 calc R . . H54C H 0.2105 -0.1252 0.3348 0.118 Uiso 1 1 calc R . . C55 C 0.5737(2) -0.0128(2) 0.42850(19) 0.0831(12) Uani 1 1 d . . . H55A H 0.5787 0.0314 0.4523 0.125 Uiso 1 1 calc R . . H55B H 0.6212 -0.0180 0.4005 0.125 Uiso 1 1 calc R . . H55C H 0.5731 -0.0518 0.4592 0.125 Uiso 1 1 calc R . . C56 C 0.4489(2) 0.30165(15) 0.27609(16) 0.0607(7) Uani 1 1 d . . . H56A H 0.4123 0.3229 0.3075 0.091 Uiso 1 1 calc R . . H56B H 0.4543 0.3333 0.2392 0.091 Uiso 1 1 calc R . . H56C H 0.5040 0.2933 0.2966 0.091 Uiso 1 1 calc R . . C57 C 0.3677(2) 0.2495(2) 0.04449(16) 0.0791(10) Uani 1 1 d . . . H57A H 0.3449 0.2930 0.0615 0.119 Uiso 1 1 calc R . . H57B H 0.3573 0.2477 -0.0025 0.119 Uiso 1 1 calc R . . H57C H 0.4279 0.2478 0.0542 0.119 Uiso 1 1 calc R . . C58 C 0.2336(2) 0.18457(19) 0.05275(15) 0.0704(9) Uani 1 1 d . . . H58A H 0.2057 0.2274 0.0664 0.106 Uiso 1 1 calc R . . H58B H 0.2061 0.1438 0.0713 0.106 Uiso 1 1 calc R . . H58C H 0.2304 0.1813 0.0054 0.106 Uiso 1 1 calc R . . C59 C 0.3679(3) 0.1179(2) 0.05417(16) 0.0935(14) Uani 1 1 d . . . H59A H 0.3668 0.1160 0.0068 0.140 Uiso 1 1 calc R . . H59B H 0.3380 0.0774 0.0709 0.140 Uiso 1 1 calc R . . H59C H 0.4259 0.1170 0.0708 0.140 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 0.03590(7) 0.03085(7) 0.05745(9) -0.00097(5) -0.01475(6) 0.00207(5) La2 0.03288(7) 0.02948(7) 0.03867(7) -0.00087(4) -0.01139(5) -0.00213(4) O1 0.0585(12) 0.0551(11) 0.0617(12) -0.0102(9) -0.0004(9) 0.0141(9) O2 0.0370(8) 0.0453(9) 0.0566(10) 0.0022(8) -0.0138(7) 0.0034(7) O21 0.0450(9) 0.0367(8) 0.0537(10) -0.0076(7) -0.0008(8) -0.0058(7) O22 0.0368(8) 0.0360(8) 0.0446(8) -0.0011(7) -0.0103(6) -0.0025(6) O41 0.0399(8) 0.0402(9) 0.0517(10) 0.0089(7) -0.0146(7) -0.0050(7) O42 0.0426(8) 0.0333(8) 0.0412(8) 0.0018(6) -0.0106(7) -0.0029(6) N1 0.0694(16) 0.0435(13) 0.100(2) -0.0205(13) -0.0420(15) 0.0178(12) N2 0.0416(11) 0.0384(11) 0.0935(18) 0.0113(11) -0.0083(11) -0.0020(9) N21 0.0424(10) 0.0294(9) 0.0479(11) -0.0012(8) -0.0126(8) -0.0044(8) N22 0.0446(11) 0.0331(9) 0.0451(10) -0.0023(8) -0.0144(8) -0.0023(8) N41 0.0392(10) 0.0473(11) 0.0500(11) 0.0018(9) -0.0167(9) -0.0076(9) N42 0.0471(11) 0.0382(10) 0.0445(11) -0.0058(8) -0.0125(9) -0.0060(8) C1 0.071(2) 0.114(3) 0.067(2) -0.001(2) 0.0109(17) 0.039(2) C2 0.0676(19) 0.081(2) 0.0512(15) -0.0029(15) -0.0066(14) 0.0395(17) C3 0.105(3) 0.080(2) 0.0632(19) -0.0241(17) -0.0173(19) 0.055(2) C4 0.092(3) 0.062(2) 0.091(2) -0.0288(18) -0.050(2) 0.0365(19) C5 0.067(2) 0.0518(18) 0.167(4) -0.028(2) -0.061(2) 0.0059(16) C6 0.0571(19) 0.0415(16) 0.181(5) -0.006(2) -0.034(2) -0.0055(14) C7 0.0467(16) 0.0397(15) 0.159(4) 0.0097(19) -0.008(2) -0.0057(12) C8 0.0436(13) 0.0435(13) 0.0586(15) 0.0119(11) 0.0092(11) 0.0102(10) C9 0.0369(12) 0.0540(15) 0.0510(14) 0.0057(11) -0.0035(10) 0.0100(10) C10 0.0338(11) 0.0514(13) 0.0378(11) 0.0000(10) -0.0030(9) 0.0055(9) C11 0.0422(13) 0.0589(16) 0.0582(15) -0.0165(13) -0.0180(11) 0.0144(11) C12 0.141(5) 0.231(8) 0.100(4) -0.025(4) 0.055(4) 0.035(5) C13 0.063(2) 0.120(4) 0.110(3) 0.031(3) 0.017(2) 0.014(2) C14 0.067(2) 0.142(4) 0.131(4) 0.008(3) -0.014(2) 0.041(3) C15 0.158(4) 0.078(3) 0.130(4) -0.059(3) -0.090(3) 0.058(3) C16 0.0666(18) 0.0483(15) 0.080(2) 0.0186(15) 0.0091(16) 0.0147(14) C17 0.0470(15) 0.0679(19) 0.084(2) -0.0006(16) -0.0247(15) 0.0070(13) C18 0.096(3) 0.074(2) 0.182(5) 0.042(3) -0.082(3) -0.039(2) C19 0.076(3) 0.260(7) 0.154(5) -0.157(5) -0.043(3) 0.063(4) C21 0.0495(15) 0.0434(14) 0.0751(19) -0.0104(13) 0.0109(13) -0.0069(11) C22 0.0457(13) 0.0311(11) 0.0523(13) 0.0010(10) -0.0027(10) 0.0000(9) C23 0.0486(14) 0.0388(12) 0.0532(14) -0.0060(10) -0.0011(11) 0.0021(10) C24 0.0506(13) 0.0307(11) 0.0501(13) -0.0037(9) -0.0161(11) 0.0015(9) C25 0.0480(13) 0.0298(11) 0.0553(14) -0.0022(10) -0.0141(11) -0.0075(9) C26 0.0488(14) 0.0419(13) 0.0553(14) -0.0101(11) -0.0196(11) -0.0058(10) C27 0.0522(14) 0.0407(12) 0.0477(13) -0.0030(10) -0.0200(11) -0.0012(10) C28 0.0387(11) 0.0320(11) 0.0544(13) 0.0000(10) -0.0167(10) -0.0006(9) C29 0.0360(11) 0.0391(12) 0.0511(13) 0.0009(10) -0.0085(10) -0.0015(9) C30 0.0339(11) 0.0345(11) 0.0456(12) -0.0011(9) -0.0094(9) 0.0052(8) C31 0.0413(12) 0.0446(13) 0.0457(12) -0.0029(10) -0.0077(10) 0.0030(10) C32 0.066(2) 0.091(3) 0.135(4) -0.047(3) 0.035(2) -0.020(2) C33 0.0518(19) 0.119(4) 0.125(4) -0.001(3) -0.021(2) -0.010(2) C34 0.088(3) 0.0442(17) 0.170(4) -0.010(2) 0.050(3) -0.0169(17) C35 0.0668(18) 0.0418(14) 0.0677(18) -0.0172(13) -0.0129(14) 0.0005(12) C36 0.0481(14) 0.0565(16) 0.0683(18) -0.0043(13) -0.0174(13) -0.0160(12) C37 0.0719(19) 0.0474(15) 0.0560(16) -0.0099(12) -0.0077(14) 0.0013(13) C38 0.0504(15) 0.080(2) 0.0462(14) 0.0031(13) -0.0117(12) 0.0111(14) C39 0.0584(16) 0.0593(17) 0.0534(15) -0.0033(13) 0.0029(13) -0.0017(13) C41 0.0421(13) 0.0403(13) 0.0689(17) 0.0151(12) -0.0069(12) 0.0017(10) C42 0.0372(11) 0.0406(12) 0.0494(13) 0.0069(10) -0.0055(10) 0.0028(9) C43 0.0452(13) 0.0532(15) 0.0611(16) 0.0172(13) -0.0188(12) 0.0000(11) C44 0.0401(13) 0.0586(16) 0.0572(15) 0.0065(12) -0.0201(11) -0.0037(11) C45 0.0442(13) 0.0573(16) 0.0630(16) 0.0063(13) -0.0218(12) -0.0153(12) C46 0.0727(19) 0.0584(17) 0.0590(17) -0.0016(13) -0.0320(15) -0.0214(14) C47 0.0677(17) 0.0523(15) 0.0458(14) -0.0092(12) -0.0139(12) -0.0107(13) C48 0.0408(12) 0.0375(12) 0.0547(14) -0.0060(10) -0.0073(10) -0.0050(9) C49 0.0421(12) 0.0376(12) 0.0504(13) 0.0022(10) -0.0029(10) -0.0043(9) C50 0.0436(12) 0.0344(11) 0.0437(12) 0.0034(9) -0.0063(10) 0.0052(9) C51 0.0613(16) 0.0491(14) 0.0430(13) 0.0052(11) -0.0093(11) 0.0011(12) C52 0.084(2) 0.067(2) 0.079(2) 0.0331(17) -0.0126(18) -0.0154(17) C53 0.076(2) 0.0438(15) 0.088(2) 0.0051(15) -0.0127(17) -0.0018(14) C54 0.0449(16) 0.0519(17) 0.140(3) 0.0304(19) 0.0070(18) -0.0008(13) C55 0.0603(19) 0.092(3) 0.093(3) 0.032(2) -0.0457(18) -0.0177(18) C56 0.0687(18) 0.0426(14) 0.0700(18) -0.0094(13) -0.0085(14) -0.0171(13) C57 0.085(2) 0.098(3) 0.0541(17) 0.0217(17) -0.0024(16) -0.022(2) C58 0.077(2) 0.080(2) 0.0523(16) 0.0159(15) -0.0268(15) -0.0162(17) C59 0.145(4) 0.088(3) 0.0460(17) -0.0099(17) -0.006(2) 0.043(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O2 2.3193(17) . ? La1 O1 2.356(2) . ? La1 N1 2.538(2) . ? La1 O42 2.5509(17) . ? La1 O22 2.5808(15) . ? La1 N2 2.606(2) . ? La1 N22 2.7940(19) . ? La1 C30 3.111(2) . ? La1 La2 3.9718(3) . ? La2 O21 2.3416(18) . ? La2 O41 2.3489(16) . ? La2 O22 2.5625(16) . ? La2 O42 2.5671(15) . ? La2 N41 2.6678(19) . ? La2 N21 2.6989(19) . ? La2 N42 2.7162(19) . ? La2 N22 2.8838(19) . ? O1 C2 1.292(3) . ? O2 C10 1.297(3) . ? O21 C22 1.290(3) . ? O22 C30 1.308(3) . ? O41 C42 1.287(3) . ? O42 C50 1.333(3) . ? N1 C4 1.280(5) . ? N1 C5 1.493(5) . ? N2 C8 1.295(3) . ? N2 C7 1.468(4) . ? N21 C24 1.301(3) . ? N21 C25 1.475(3) . ? N22 C28 1.303(3) . ? N22 C27 1.475(3) . ? N41 C44 1.299(3) . ? N41 C45 1.472(3) . ? N42 C48 1.288(3) . ? N42 C47 1.471(3) . ? C1 C13 1.522(6) . ? C1 C12 1.526(5) . ? C1 C2 1.527(6) . ? C1 C14 1.539(5) . ? C2 C3 1.389(5) . ? C3 C4 1.431(6) . ? C4 C15 1.534(5) . ? C5 C6 1.507(6) . ? C6 C7 1.495(6) . ? C8 C9 1.433(4) . ? C8 C16 1.521(4) . ? C9 C10 1.363(4) . ? C10 C11 1.533(3) . ? C11 C19 1.511(5) . ? C11 C18 1.514(5) . ? C11 C17 1.517(4) . ? C21 C34 1.500(4) . ? C21 C32 1.505(4) . ? C21 C22 1.541(4) . ? C21 C33 1.543(5) . ? C22 C23 1.370(3) . ? C23 C24 1.432(4) . ? C24 C35 1.527(3) . ? C25 C26 1.524(3) . ? C26 C27 1.528(3) . ? C28 C29 1.441(3) . ? C28 C36 1.515(3) . ? C29 C30 1.381(3) . ? C30 C31 1.533(3) . ? C31 C37 1.529(4) . ? C31 C39 1.531(4) . ? C31 C38 1.539(3) . ? C41 C52 1.516(4) . ? C41 C54 1.529(4) . ? C41 C42 1.537(3) . ? C41 C53 1.540(4) . ? C42 C43 1.365(3) . ? C43 C44 1.431(4) . ? C44 C55 1.532(3) . ? C45 C46 1.519(4) . ? C46 C47 1.527(4) . ? C48 C49 1.448(3) . ? C48 C56 1.522(3) . ? C49 C50 1.356(3) . ? C50 C51 1.534(3) . ? C51 C58 1.518(4) . ? C51 C57 1.529(4) . ? C51 C59 1.538(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La1 O1 82.70(7) . . ? O2 La1 N1 127.94(7) . . ? O1 La1 N1 69.96(9) . . ? O2 La1 O42 98.66(6) . . ? O1 La1 O42 173.93(6) . . ? N1 La1 O42 113.14(8) . . ? O2 La1 O22 139.50(5) . . ? O1 La1 O22 99.84(6) . . ? N1 La1 O22 89.60(7) . . ? O42 La1 O22 75.25(5) . . ? O2 La1 N2 72.15(7) . . ? O1 La1 N2 98.19(7) . . ? N1 La1 N2 69.21(9) . . ? O42 La1 N2 87.85(6) . . ? O22 La1 N2 145.29(6) . . ? O2 La1 N22 77.09(6) . . ? O1 La1 N22 106.80(7) . . ? N1 La1 N22 152.27(7) . . ? O42 La1 N22 67.93(6) . . ? O22 La1 N22 63.38(5) . . ? N2 La1 N22 137.14(7) . . ? O2 La1 C30 124.81(6) . . ? O1 La1 C30 78.14(7) . . ? N1 La1 C30 92.47(8) . . ? O42 La1 C30 96.33(5) . . ? O22 La1 C30 24.37(5) . . ? N2 La1 C30 161.28(7) . . ? N22 La1 C30 60.45(6) . . ? O2 La1 La2 115.19(4) . . ? O1 La1 La2 134.92(5) . . ? N1 La1 La2 115.50(5) . . ? O42 La1 La2 39.25(3) . . ? O22 La1 La2 39.28(4) . . ? N2 La1 La2 126.24(5) . . ? N22 La1 La2 46.54(4) . . ? C30 La1 La2 57.41(4) . . ? O21 La2 O41 115.40(6) . . ? O21 La2 O22 158.58(5) . . ? O41 La2 O22 81.34(6) . . ? O21 La2 O42 93.65(6) . . ? O41 La2 O42 146.77(5) . . ? O22 La2 O42 75.29(5) . . ? O21 La2 N41 77.62(7) . . ? O41 La2 N41 69.16(6) . . ? O22 La2 N41 97.71(6) . . ? O42 La2 N41 136.73(6) . . ? O21 La2 N21 68.20(6) . . ? O41 La2 N21 78.36(6) . . ? O22 La2 N21 131.06(5) . . ? O42 La2 N21 99.58(5) . . ? N41 La2 N21 115.31(6) . . ? O21 La2 N42 87.53(6) . . ? O41 La2 N42 127.55(6) . . ? O22 La2 N42 71.27(6) . . ? O42 La2 N42 65.98(5) . . ? N41 La2 N42 71.31(6) . . ? N21 La2 N42 151.43(6) . . ? O21 La2 N22 130.30(6) . . ? O41 La2 N22 82.05(6) . . ? O22 La2 N22 62.27(5) . . ? O42 La2 N22 66.31(5) . . ? N41 La2 N22 147.53(6) . . ? N21 La2 N22 71.08(6) . . ? N42 La2 N22 119.42(6) . . ? O21 La2 La1 132.60(4) . . ? O41 La2 La1 110.12(4) . . ? O22 La2 La1 39.62(3) . . ? O42 La2 La1 38.95(4) . . ? N41 La2 La1 132.78(5) . . ? N21 La2 La1 110.30(4) . . ? N42 La2 La1 74.73(4) . . ? N22 La2 La1 44.69(4) . . ? C2 O1 La1 142.1(2) . . ? C10 O2 La1 130.34(16) . . ? C22 O21 La2 145.07(15) . . ? C30 O22 La2 125.21(14) . . ? C30 O22 La1 101.14(12) . . ? La2 O22 La1 101.11(6) . . ? C42 O41 La2 143.41(15) . . ? C50 O42 La1 134.74(14) . . ? C50 O42 La2 116.68(13) . . ? La1 O42 La2 101.80(6) . . ? C4 N1 C5 119.4(3) . . ? C4 N1 La1 135.1(3) . . ? C5 N1 La1 105.2(2) . . ? C8 N2 C7 119.5(2) . . ? C8 N2 La1 123.66(17) . . ? C7 N2 La1 116.32(19) . . ? C24 N21 C25 117.6(2) . . ? C24 N21 La2 131.70(15) . . ? C25 N21 La2 110.56(15) . . ? C28 N22 C27 120.0(2) . . ? C28 N22 La1 93.82(14) . . ? C27 N22 La1 114.65(14) . . ? C28 N22 La2 122.85(14) . . ? C27 N22 La2 110.11(15) . . ? La1 N22 La2 88.76(5) . . ? C44 N41 C45 118.7(2) . . ? C44 N41 La2 130.54(16) . . ? C45 N41 La2 110.18(15) . . ? C48 N42 C47 120.3(2) . . ? C48 N42 La2 126.70(16) . . ? C47 N42 La2 112.53(16) . . ? C13 C1 C12 109.9(4) . . ? C13 C1 C2 110.1(3) . . ? C12 C1 C2 113.7(4) . . ? C13 C1 C14 108.4(4) . . ? C12 C1 C14 107.7(4) . . ? C2 C1 C14 106.8(3) . . ? O1 C2 C3 122.5(3) . . ? O1 C2 C1 114.7(3) . . ? C3 C2 C1 122.6(3) . . ? C2 C3 C4 126.9(3) . . ? N1 C4 C3 123.2(3) . . ? N1 C4 C15 123.0(4) . . ? C3 C4 C15 113.8(4) . . ? N1 C5 C6 112.5(3) . . ? C7 C6 C5 113.8(3) . . ? N2 C7 C6 113.9(3) . . ? N2 C8 C9 124.0(2) . . ? N2 C8 C16 122.7(3) . . ? C9 C8 C16 113.3(2) . . ? C10 C9 C8 128.4(2) . . ? O2 C10 C9 124.1(2) . . ? O2 C10 C11 114.3(2) . . ? C9 C10 C11 121.6(2) . . ? C19 C11 C18 108.6(4) . . ? C19 C11 C17 109.0(3) . . ? C18 C11 C17 108.1(3) . . ? C19 C11 C10 107.6(3) . . ? C18 C11 C10 108.6(2) . . ? C17 C11 C10 114.8(2) . . ? C34 C21 C32 110.5(3) . . ? C34 C21 C22 109.7(3) . . ? C32 C21 C22 114.1(3) . . ? C34 C21 C33 108.3(3) . . ? C32 C21 C33 108.3(3) . . ? C22 C21 C33 105.7(3) . . ? O21 C22 C23 123.9(2) . . ? O21 C22 C21 114.8(2) . . ? C23 C22 C21 121.2(2) . . ? C22 C23 C24 126.7(2) . . ? N21 C24 C23 124.0(2) . . ? N21 C24 C35 122.7(2) . . ? C23 C24 C35 113.3(2) . . ? N21 C25 C26 112.9(2) . . ? C25 C26 C27 112.50(19) . . ? N22 C27 C26 115.1(2) . . ? N22 C28 C29 122.4(2) . . ? N22 C28 C36 123.7(2) . . ? C29 C28 C36 113.9(2) . . ? C30 C29 C28 127.8(2) . . ? O22 C30 C29 122.4(2) . . ? O22 C30 C31 115.85(19) . . ? C29 C30 C31 121.7(2) . . ? O22 C30 La1 54.49(10) . . ? C29 C30 La1 83.91(14) . . ? C31 C30 La1 133.38(15) . . ? C37 C31 C39 109.3(2) . . ? C37 C31 C30 108.9(2) . . ? C39 C31 C30 113.8(2) . . ? C37 C31 C38 108.9(2) . . ? C39 C31 C38 108.1(2) . . ? C30 C31 C38 107.8(2) . . ? C52 C41 C54 110.1(3) . . ? C52 C41 C42 114.4(2) . . ? C54 C41 C42 109.3(2) . . ? C52 C41 C53 108.6(3) . . ? C54 C41 C53 108.0(3) . . ? C42 C41 C53 106.1(2) . . ? O41 C42 C43 123.5(2) . . ? O41 C42 C41 115.4(2) . . ? C43 C42 C41 121.0(2) . . ? C42 C43 C44 127.7(2) . . ? N41 C44 C43 124.3(2) . . ? N41 C44 C55 122.2(3) . . ? C43 C44 C55 113.5(2) . . ? N41 C45 C46 112.2(2) . . ? C45 C46 C47 112.9(2) . . ? N42 C47 C46 111.3(2) . . ? N42 C48 C49 121.0(2) . . ? N42 C48 C56 124.2(2) . . ? C49 C48 C56 114.8(2) . . ? C50 C49 C48 127.6(2) . . ? O42 C50 C49 123.1(2) . . ? O42 C50 C51 115.6(2) . . ? C49 C50 C51 121.3(2) . . ? C58 C51 C57 108.4(2) . . ? C58 C51 C50 111.7(2) . . ? C57 C51 C50 113.1(2) . . ? C58 C51 C59 108.4(3) . . ? C57 C51 C59 109.0(3) . . ? C50 C51 C59 106.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 La1 La2 O21 70.46(7) . . . . ? O1 La1 La2 O21 176.16(9) . . . . ? N1 La1 La2 O21 -97.30(10) . . . . ? O42 La1 La2 O21 -1.31(7) . . . . ? O22 La1 La2 O21 -150.76(8) . . . . ? N2 La1 La2 O21 -15.23(9) . . . . ? N22 La1 La2 O21 108.66(8) . . . . ? C30 La1 La2 O21 -172.92(7) . . . . ? O2 La1 La2 O41 -92.76(7) . . . . ? O1 La1 La2 O41 12.95(8) . . . . ? N1 La1 La2 O41 99.48(10) . . . . ? O42 La1 La2 O41 -164.53(7) . . . . ? O22 La1 La2 O41 46.03(7) . . . . ? N2 La1 La2 O41 -178.44(8) . . . . ? N22 La1 La2 O41 -54.56(7) . . . . ? C30 La1 La2 O41 23.86(7) . . . . ? O2 La1 La2 O22 -138.79(7) . . . . ? O1 La1 La2 O22 -33.08(9) . . . . ? N1 La1 La2 O22 53.45(10) . . . . ? O42 La1 La2 O22 149.44(8) . . . . ? N2 La1 La2 O22 135.53(9) . . . . ? N22 La1 La2 O22 -100.58(8) . . . . ? C30 La1 La2 O22 -22.17(7) . . . . ? O2 La1 La2 O42 71.77(7) . . . . ? O1 La1 La2 O42 177.48(9) . . . . ? N1 La1 La2 O42 -95.99(10) . . . . ? O22 La1 La2 O42 -149.44(8) . . . . ? N2 La1 La2 O42 -13.91(9) . . . . ? N22 La1 La2 O42 109.98(8) . . . . ? C30 La1 La2 O42 -171.61(7) . . . . ? O2 La1 La2 N41 -172.55(8) . . . . ? O1 La1 La2 N41 -66.85(9) . . . . ? N1 La1 La2 N41 19.69(11) . . . . ? O42 La1 La2 N41 115.68(8) . . . . ? O22 La1 La2 N41 -33.77(8) . . . . ? N2 La1 La2 N41 101.76(10) . . . . ? N22 La1 La2 N41 -134.35(9) . . . . ? C30 La1 La2 N41 -55.93(8) . . . . ? O2 La1 La2 N21 -8.13(7) . . . . ? O1 La1 La2 N21 97.58(8) . . . . ? N1 La1 La2 N21 -175.89(10) . . . . ? O42 La1 La2 N21 -79.90(7) . . . . ? O22 La1 La2 N21 130.66(7) . . . . ? N2 La1 La2 N21 -93.81(9) . . . . ? N22 La1 La2 N21 30.08(7) . . . . ? C30 La1 La2 N21 108.49(7) . . . . ? O2 La1 La2 N42 142.29(7) . . . . ? O1 La1 La2 N42 -112.00(8) . . . . ? N1 La1 La2 N42 -25.47(10) . . . . ? O42 La1 La2 N42 70.52(7) . . . . ? O22 La1 La2 N42 -78.92(7) . . . . ? N2 La1 La2 N42 56.61(9) . . . . ? N22 La1 La2 N42 -179.50(7) . . . . ? C30 La1 La2 N42 -101.08(7) . . . . ? O2 La1 La2 N22 -38.20(8) . . . . ? O1 La1 La2 N22 67.50(9) . . . . ? N1 La1 La2 N22 154.03(10) . . . . ? O42 La1 La2 N22 -109.98(8) . . . . ? O22 La1 La2 N22 100.58(8) . . . . ? N2 La1 La2 N22 -123.89(9) . . . . ? C30 La1 La2 N22 78.42(8) . . . . ? O2 La1 O1 C2 -138.4(3) . . . . ? N1 La1 O1 C2 -3.4(3) . . . . ? O42 La1 O1 C2 118.3(6) . . . . ? O22 La1 O1 C2 82.5(3) . . . . ? N2 La1 O1 C2 -67.7(3) . . . . ? N22 La1 O1 C2 147.5(3) . . . . ? C30 La1 O1 C2 93.7(3) . . . . ? La2 La1 O1 C2 103.0(3) . . . . ? O1 La1 O2 C10 58.5(2) . . . . ? N1 La1 O2 C10 1.1(3) . . . . ? O42 La1 O2 C10 -127.5(2) . . . . ? O22 La1 O2 C10 155.15(18) . . . . ? N2 La1 O2 C10 -42.6(2) . . . . ? N22 La1 O2 C10 167.7(2) . . . . ? C30 La1 O2 C10 128.6(2) . . . . ? La2 La1 O2 C10 -164.89(19) . . . . ? O41 La2 O21 C22 60.9(3) . . . . ? O22 La2 O21 C22 -160.2(2) . . . . ? O42 La2 O21 C22 -102.5(3) . . . . ? N41 La2 O21 C22 120.4(3) . . . . ? N21 La2 O21 C22 -3.6(3) . . . . ? N42 La2 O21 C22 -168.2(3) . . . . ? N22 La2 O21 C22 -40.8(3) . . . . ? La1 La2 O21 C22 -101.6(3) . . . . ? O21 La2 O22 C30 -167.67(17) . . . . ? O41 La2 O22 C30 -24.58(16) . . . . ? O42 La2 O22 C30 131.60(16) . . . . ? N41 La2 O22 C30 -92.01(16) . . . . ? N21 La2 O22 C30 41.63(18) . . . . ? N42 La2 O22 C30 -159.22(17) . . . . ? N22 La2 O22 C30 60.95(16) . . . . ? La1 La2 O22 C30 112.30(17) . . . . ? O21 La2 O22 La1 80.03(16) . . . . ? O41 La2 O22 La1 -136.88(6) . . . . ? O42 La2 O22 La1 19.30(5) . . . . ? N41 La2 O22 La1 155.69(6) . . . . ? N21 La2 O22 La1 -70.67(8) . . . . ? N42 La2 O22 La1 88.48(6) . . . . ? N22 La2 O22 La1 -51.35(5) . . . . ? O2 La1 O22 C30 -62.96(16) . . . . ? O1 La1 O22 C30 27.30(14) . . . . ? N1 La1 O22 C30 96.87(15) . . . . ? O42 La1 O22 C30 -149.04(14) . . . . ? N2 La1 O22 C30 147.58(15) . . . . ? N22 La1 O22 C30 -76.66(14) . . . . ? La2 La1 O22 C30 -129.61(15) . . . . ? O2 La1 O22 La2 66.65(10) . . . . ? O1 La1 O22 La2 156.90(6) . . . . ? N1 La1 O22 La2 -133.52(9) . . . . ? O42 La1 O22 La2 -19.43(5) . . . . ? N2 La1 O22 La2 -82.81(13) . . . . ? N22 La1 O22 La2 52.95(6) . . . . ? C30 La1 O22 La2 129.61(15) . . . . ? O21 La2 O41 C42 51.9(3) . . . . ? O22 La2 O41 C42 -114.1(3) . . . . ? O42 La2 O41 C42 -159.6(2) . . . . ? N41 La2 O41 C42 -12.4(3) . . . . ? N21 La2 O41 C42 110.7(3) . . . . ? N42 La2 O41 C42 -55.9(3) . . . . ? N22 La2 O41 C42 -177.1(3) . . . . ? La1 La2 O41 C42 -141.7(3) . . . . ? O2 La1 O42 C50 91.9(2) . . . . ? O1 La1 O42 C50 -165.7(5) . . . . ? N1 La1 O42 C50 -46.0(2) . . . . ? O22 La1 O42 C50 -129.1(2) . . . . ? N2 La1 O42 C50 20.3(2) . . . . ? N22 La1 O42 C50 164.1(2) . . . . ? C30 La1 O42 C50 -141.43(19) . . . . ? La2 La1 O42 C50 -148.5(2) . . . . ? O2 La1 O42 La2 -119.61(6) . . . . ? O1 La1 O42 La2 -17.1(6) . . . . ? N1 La1 O42 La2 102.53(8) . . . . ? O22 La1 O42 La2 19.44(5) . . . . ? N2 La1 O42 La2 168.81(7) . . . . ? N22 La1 O42 La2 -47.41(5) . . . . ? C30 La1 O42 La2 7.11(6) . . . . ? O21 La2 O42 C50 -25.49(16) . . . . ? O41 La2 O42 C50 -177.32(15) . . . . ? O22 La2 O42 C50 135.90(16) . . . . ? N41 La2 O42 C50 50.29(19) . . . . ? N21 La2 O42 C50 -93.97(16) . . . . ? N42 La2 O42 C50 60.17(15) . . . . ? N22 La2 O42 C50 -158.31(17) . . . . ? La1 La2 O42 C50 155.48(18) . . . . ? O21 La2 O42 La1 179.03(5) . . . . ? O41 La2 O42 La1 27.19(12) . . . . ? O22 La2 O42 La1 -19.58(5) . . . . ? N41 La2 O42 La1 -105.19(9) . . . . ? N21 La2 O42 La1 110.54(6) . . . . ? N42 La2 O42 La1 -95.31(7) . . . . ? N22 La2 O42 La1 46.20(6) . . . . ? O2 La1 N1 C4 64.7(3) . . . . ? O1 La1 N1 C4 1.8(3) . . . . ? O42 La1 N1 C4 -172.6(3) . . . . ? O22 La1 N1 C4 -98.8(3) . . . . ? N2 La1 N1 C4 109.3(3) . . . . ? N22 La1 N1 C4 -86.3(3) . . . . ? C30 La1 N1 C4 -74.6(3) . . . . ? La2 La1 N1 C4 -129.4(3) . . . . ? O2 La1 N1 C5 -109.70(19) . . . . ? O1 La1 N1 C5 -172.6(2) . . . . ? O42 La1 N1 C5 13.0(2) . . . . ? O22 La1 N1 C5 86.8(2) . . . . ? N2 La1 N1 C5 -65.1(2) . . . . ? N22 La1 N1 C5 99.3(3) . . . . ? C30 La1 N1 C5 111.0(2) . . . . ? La2 La1 N1 C5 56.2(2) . . . . ? O2 La1 N2 C8 34.0(2) . . . . ? O1 La1 N2 C8 -45.5(2) . . . . ? N1 La1 N2 C8 -110.4(3) . . . . ? O42 La1 N2 C8 133.8(2) . . . . ? O22 La1 N2 C8 -166.27(19) . . . . ? N22 La1 N2 C8 80.2(3) . . . . ? C30 La1 N2 C8 -122.7(3) . . . . ? La2 La1 N2 C8 142.6(2) . . . . ? O2 La1 N2 C7 -154.2(3) . . . . ? O1 La1 N2 C7 126.2(2) . . . . ? N1 La1 N2 C7 61.4(2) . . . . ? O42 La1 N2 C7 -54.4(2) . . . . ? O22 La1 N2 C7 5.5(3) . . . . ? N22 La1 N2 C7 -108.0(2) . . . . ? C30 La1 N2 C7 49.1(4) . . . . ? La2 La1 N2 C7 -45.6(3) . . . . ? O21 La2 N21 C24 -1.9(2) . . . . ? O41 La2 N21 C24 -125.5(2) . . . . ? O22 La2 N21 C24 167.03(19) . . . . ? O42 La2 N21 C24 88.2(2) . . . . ? N41 La2 N21 C24 -65.5(2) . . . . ? N42 La2 N21 C24 31.8(3) . . . . ? N22 La2 N21 C24 149.0(2) . . . . ? La1 La2 N21 C24 127.1(2) . . . . ? O21 La2 N21 C25 174.31(16) . . . . ? O41 La2 N21 C25 50.66(14) . . . . ? O22 La2 N21 C25 -16.79(17) . . . . ? O42 La2 N21 C25 -95.58(14) . . . . ? N41 La2 N21 C25 110.71(14) . . . . ? N42 La2 N21 C25 -151.98(14) . . . . ? N22 La2 N21 C25 -34.82(14) . . . . ? La1 La2 N21 C25 -56.70(14) . . . . ? O2 La1 N22 C28 -92.20(14) . . . . ? O1 La1 N22 C28 -14.05(15) . . . . ? N1 La1 N22 C28 64.7(2) . . . . ? O42 La1 N22 C28 162.76(14) . . . . ? O22 La1 N22 C28 78.73(13) . . . . ? N2 La1 N22 C28 -137.01(14) . . . . ? C30 La1 N22 C28 51.24(13) . . . . ? La2 La1 N22 C28 122.84(15) . . . . ? O2 La1 N22 C27 33.34(16) . . . . ? O1 La1 N22 C27 111.49(17) . . . . ? N1 La1 N22 C27 -169.8(2) . . . . ? O42 La1 N22 C27 -71.71(16) . . . . ? O22 La1 N22 C27 -155.74(18) . . . . ? N2 La1 N22 C27 -11.5(2) . . . . ? C30 La1 N22 C27 176.78(18) . . . . ? La2 La1 N22 C27 -111.62(18) . . . . ? O2 La1 N22 La2 144.96(7) . . . . ? O1 La1 N22 La2 -136.89(6) . . . . ? N1 La1 N22 La2 -58.14(19) . . . . ? O42 La1 N22 La2 39.91(5) . . . . ? O22 La1 N22 La2 -44.11(5) . . . . ? N2 La1 N22 La2 100.15(9) . . . . ? C30 La1 N22 La2 -71.60(6) . . . . ? O21 La2 N22 C28 152.39(17) . . . . ? O41 La2 N22 C28 35.69(18) . . . . ? O22 La2 N22 C28 -48.66(17) . . . . ? O42 La2 N22 C28 -133.93(19) . . . . ? N41 La2 N22 C28 8.4(2) . . . . ? N21 La2 N22 C28 116.05(19) . . . . ? N42 La2 N22 C28 -93.19(18) . . . . ? La1 La2 N22 C28 -93.74(18) . . . . ? O21 La2 N22 C27 2.01(17) . . . . ? O41 La2 N22 C27 -114.69(15) . . . . ? O22 La2 N22 C27 160.95(16) . . . . ? O42 La2 N22 C27 75.69(14) . . . . ? N41 La2 N22 C27 -141.99(15) . . . . ? N21 La2 N22 C27 -34.34(14) . . . . ? N42 La2 N22 C27 116.43(14) . . . . ? La1 La2 N22 C27 115.87(16) . . . . ? O21 La2 N22 La1 -113.87(7) . . . . ? O41 La2 N22 La1 129.43(6) . . . . ? O22 La2 N22 La1 45.08(5) . . . . ? O42 La2 N22 La1 -40.18(5) . . . . ? N41 La2 N22 La1 102.14(11) . . . . ? N21 La2 N22 La1 -150.21(7) . . . . ? N42 La2 N22 La1 0.55(8) . . . . ? O21 La2 N41 C44 -112.3(3) . . . . ? O41 La2 N41 C44 11.3(2) . . . . ? O22 La2 N41 C44 89.0(3) . . . . ? O42 La2 N41 C44 165.7(2) . . . . ? N21 La2 N41 C44 -53.9(3) . . . . ? N42 La2 N41 C44 156.1(3) . . . . ? N22 La2 N41 C44 40.4(3) . . . . ? La1 La2 N41 C44 109.9(2) . . . . ? O21 La2 N41 C45 58.28(18) . . . . ? O41 La2 N41 C45 -178.1(2) . . . . ? O22 La2 N41 C45 -100.49(18) . . . . ? O42 La2 N41 C45 -23.8(2) . . . . ? N21 La2 N41 C45 116.64(18) . . . . ? N42 La2 N41 C45 -33.31(18) . . . . ? N22 La2 N41 C45 -149.04(16) . . . . ? La1 La2 N41 C45 -79.53(19) . . . . ? O21 La2 N42 C48 55.2(2) . . . . ? O41 La2 N42 C48 175.79(19) . . . . ? O22 La2 N42 C48 -121.7(2) . . . . ? O42 La2 N42 C48 -39.9(2) . . . . ? N41 La2 N42 C48 133.0(2) . . . . ? N21 La2 N42 C48 24.2(3) . . . . ? N22 La2 N42 C48 -80.7(2) . . . . ? La1 La2 N42 C48 -80.3(2) . . . . ? O21 La2 N42 C47 -116.54(18) . . . . ? O41 La2 N42 C47 4.0(2) . . . . ? O22 La2 N42 C47 66.54(17) . . . . ? O42 La2 N42 C47 148.36(19) . . . . ? N41 La2 N42 C47 -38.78(17) . . . . ? N21 La2 N42 C47 -147.59(17) . . . . ? N22 La2 N42 C47 107.50(17) . . . . ? La1 La2 N42 C47 107.90(18) . . . . ? La1 O1 C2 C3 2.2(5) . . . . ? La1 O1 C2 C1 178.7(2) . . . . ? C13 C1 C2 O1 36.9(4) . . . . ? C12 C1 C2 O1 160.7(4) . . . . ? C14 C1 C2 O1 -80.6(4) . . . . ? C13 C1 C2 C3 -146.7(3) . . . . ? C12 C1 C2 C3 -22.9(5) . . . . ? C14 C1 C2 C3 95.8(4) . . . . ? O1 C2 C3 C4 2.4(5) . . . . ? C1 C2 C3 C4 -173.7(3) . . . . ? C5 N1 C4 C3 174.3(3) . . . . ? La1 N1 C4 C3 0.5(5) . . . . ? C5 N1 C4 C15 -6.6(5) . . . . ? La1 N1 C4 C15 179.6(2) . . . . ? C2 C3 C4 N1 -3.5(6) . . . . ? C2 C3 C4 C15 177.3(3) . . . . ? C4 N1 C5 C6 -86.5(4) . . . . ? La1 N1 C5 C6 89.0(3) . . . . ? N1 C5 C6 C7 -73.9(4) . . . . ? C8 N2 C7 C6 104.7(4) . . . . ? La1 N2 C7 C6 -67.4(3) . . . . ? C5 C6 C7 N2 58.9(4) . . . . ? C7 N2 C8 C9 170.3(3) . . . . ? La1 N2 C8 C9 -18.2(4) . . . . ? C7 N2 C8 C16 -7.2(5) . . . . ? La1 N2 C8 C16 164.3(2) . . . . ? N2 C8 C9 C10 -13.1(5) . . . . ? C16 C8 C9 C10 164.6(3) . . . . ? La1 O2 C10 C9 33.3(4) . . . . ? La1 O2 C10 C11 -148.89(18) . . . . ? C8 C9 C10 O2 8.7(4) . . . . ? C8 C9 C10 C11 -168.9(3) . . . . ? O2 C10 C11 C19 -65.0(4) . . . . ? C9 C10 C11 C19 112.8(4) . . . . ? O2 C10 C11 C18 52.4(3) . . . . ? C9 C10 C11 C18 -129.8(3) . . . . ? O2 C10 C11 C17 173.5(3) . . . . ? C9 C10 C11 C17 -8.7(4) . . . . ? La2 O21 C22 C23 8.4(4) . . . . ? La2 O21 C22 C21 -169.1(2) . . . . ? C34 C21 C22 O21 -49.2(4) . . . . ? C32 C21 C22 O21 -173.7(3) . . . . ? C33 C21 C22 O21 67.4(3) . . . . ? C34 C21 C22 C23 133.3(3) . . . . ? C32 C21 C22 C23 8.8(4) . . . . ? C33 C21 C22 C23 -110.1(3) . . . . ? O21 C22 C23 C24 -7.3(4) . . . . ? C21 C22 C23 C24 170.0(3) . . . . ? C25 N21 C24 C23 -173.8(2) . . . . ? La2 N21 C24 C23 2.1(4) . . . . ? C25 N21 C24 C35 3.4(3) . . . . ? La2 N21 C24 C35 179.40(17) . . . . ? C22 C23 C24 N21 2.6(4) . . . . ? C22 C23 C24 C35 -174.9(3) . . . . ? C24 N21 C25 C26 -92.3(3) . . . . ? La2 N21 C25 C26 90.9(2) . . . . ? N21 C25 C26 C27 -56.7(3) . . . . ? C28 N22 C27 C26 -72.1(3) . . . . ? La1 N22 C27 C26 177.50(17) . . . . ? La2 N22 C27 C26 79.3(2) . . . . ? C25 C26 C27 N22 -39.9(3) . . . . ? C27 N22 C28 C29 -178.4(2) . . . . ? La1 N22 C28 C29 -57.0(2) . . . . ? La2 N22 C28 C29 34.0(3) . . . . ? C27 N22 C28 C36 1.4(4) . . . . ? La1 N22 C28 C36 122.8(2) . . . . ? La2 N22 C28 C36 -146.17(19) . . . . ? N22 C28 C29 C30 0.0(4) . . . . ? C36 C28 C29 C30 -179.9(2) . . . . ? La2 O22 C30 C29 -59.7(3) . . . . ? La1 O22 C30 C29 52.6(2) . . . . ? La2 O22 C30 C31 121.43(17) . . . . ? La1 O22 C30 C31 -126.29(16) . . . . ? La2 O22 C30 La1 -112.29(14) . . . . ? C28 C29 C30 O22 8.5(4) . . . . ? C28 C29 C30 C31 -172.6(2) . . . . ? C28 C29 C30 La1 49.1(2) . . . . ? O2 La1 C30 O22 135.21(13) . . . . ? O1 La1 C30 O22 -152.50(14) . . . . ? N1 La1 C30 O22 -83.57(14) . . . . ? O42 La1 C30 O22 30.04(13) . . . . ? N2 La1 C30 O22 -72.1(3) . . . . ? N22 La1 C30 O22 90.20(14) . . . . ? La2 La1 C30 O22 35.37(11) . . . . ? O2 La1 C30 C29 -2.37(17) . . . . ? O1 La1 C30 C29 69.92(15) . . . . ? N1 La1 C30 C29 138.85(15) . . . . ? O42 La1 C30 C29 -107.54(14) . . . . ? O22 La1 C30 C29 -137.6(2) . . . . ? N2 La1 C30 C29 150.3(2) . . . . ? N22 La1 C30 C29 -47.37(14) . . . . ? La2 La1 C30 C29 -102.21(15) . . . . ? O2 La1 C30 C31 -131.2(2) . . . . ? O1 La1 C30 C31 -58.9(2) . . . . ? N1 La1 C30 C31 10.0(2) . . . . ? O42 La1 C30 C31 123.6(2) . . . . ? O22 La1 C30 C31 93.6(2) . . . . ? N2 La1 C30 C31 21.5(3) . . . . ? N22 La1 C30 C31 -176.2(2) . . . . ? La2 La1 C30 C31 129.0(2) . . . . ? O22 C30 C31 C37 53.2(3) . . . . ? C29 C30 C31 C37 -125.7(2) . . . . ? La1 C30 C31 C37 -11.3(3) . . . . ? O22 C30 C31 C39 175.4(2) . . . . ? C29 C30 C31 C39 -3.5(3) . . . . ? La1 C30 C31 C39 110.9(2) . . . . ? O22 C30 C31 C38 -64.7(3) . . . . ? C29 C30 C31 C38 116.4(3) . . . . ? La1 C30 C31 C38 -129.3(2) . . . . ? La2 O41 C42 C43 10.1(5) . . . . ? La2 O41 C42 C41 -166.89(19) . . . . ? C52 C41 C42 O41 -162.9(3) . . . . ? C54 C41 C42 O41 -38.9(4) . . . . ? C53 C41 C42 O41 77.3(3) . . . . ? C52 C41 C42 C43 20.0(4) . . . . ? C54 C41 C42 C43 144.1(3) . . . . ? C53 C41 C42 C43 -99.7(3) . . . . ? O41 C42 C43 C44 0.2(5) . . . . ? C41 C42 C43 C44 177.0(3) . . . . ? C45 N41 C44 C43 180.0(3) . . . . ? La2 N41 C44 C43 -10.1(5) . . . . ? C45 N41 C44 C55 -1.4(5) . . . . ? La2 N41 C44 C55 168.5(2) . . . . ? C42 C43 C44 N41 1.6(5) . . . . ? C42 C43 C44 C55 -177.2(3) . . . . ? C44 N41 C45 C46 -99.8(3) . . . . ? La2 N41 C45 C46 88.4(2) . . . . ? N41 C45 C46 C47 -54.9(3) . . . . ? C48 N42 C47 C46 -89.4(3) . . . . ? La2 N42 C47 C46 83.0(2) . . . . ? C45 C46 C47 N42 -39.0(3) . . . . ? C47 N42 C48 C49 -178.4(2) . . . . ? La2 N42 C48 C49 10.4(3) . . . . ? C47 N42 C48 C56 1.2(4) . . . . ? La2 N42 C48 C56 -170.0(2) . . . . ? N42 C48 C49 C50 26.2(4) . . . . ? C56 C48 C49 C50 -153.5(3) . . . . ? La1 O42 C50 C49 85.3(3) . . . . ? La2 O42 C50 C49 -59.8(3) . . . . ? La1 O42 C50 C51 -96.5(2) . . . . ? La2 O42 C50 C51 118.40(18) . . . . ? C48 C49 C50 O42 0.9(4) . . . . ? C48 C49 C50 C51 -177.1(2) . . . . ? O42 C50 C51 C58 41.9(3) . . . . ? C49 C50 C51 C58 -139.9(3) . . . . ? O42 C50 C51 C57 164.4(2) . . . . ? C49 C50 C51 C57 -17.4(4) . . . . ? O42 C50 C51 C59 -76.1(3) . . . . ? C49 C50 C51 C59 102.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.209 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.075 data_jbj2 _database_code_CSD 212788 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Bis-5,5’-(1,3-propanediyldiimino)-2,2-dimethyl-4-hexene-3-onato] neodymium [bis(trimethylsilyl)-amido][tetrahydrofuran] ; _chemical_name_common ; (Bis-5,5’-(1,3-propanediyldiimino)-2,2-dimethyl-4-hexene-3- onato) neodymium (bis(trimethylsilyl)-amido)(tetrahydrofuran) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H58 N3 Nd O3 Si2' _chemical_formula_weight 697.20 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3066(8) _cell_length_b 15.7387(11) _cell_length_c 20.1556(14) _cell_angle_alpha 90.00 _cell_angle_beta 95.0120(10) _cell_angle_gamma 90.00 _cell_volume 3573.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4600 _cell_measurement_theta_min 2.223 _cell_measurement_theta_max 23.931 _exptl_crystal_description Chunk _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 1.550 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4053 _exptl_absorpt_correction_T_max 0.4544 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 SMART APEX CCD Area Detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 21937 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0775 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.33 _reflns_number_total 8046 _reflns_number_gt 5474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8046 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 0.857 _refine_ls_restrained_S_all 0.857 _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 Nd Nd 0.010114(16) 0.371250(14) 0.184822(9) 0.03267(7) Uani 1 1 d . . . Si1 Si -0.14548(10) 0.29491(8) 0.31180(6) 0.0434(3) Uani 1 1 d . . . Si2 Si -0.08490(12) 0.48070(8) 0.32610(6) 0.0522(3) Uani 1 1 d . . . O1 O 0.0684(2) 0.25771(18) 0.12676(13) 0.0493(7) Uani 1 1 d . . . O2 O 0.1753(2) 0.44381(18) 0.16888(14) 0.0526(8) Uani 1 1 d . . . N1 N -0.1679(2) 0.3218(2) 0.10826(15) 0.0409(8) Uani 1 1 d . . . N2 N -0.0482(2) 0.50064(19) 0.11179(15) 0.0358(8) Uani 1 1 d . . . N3 N -0.0818(2) 0.38578(18) 0.28640(14) 0.0350(7) Uani 1 1 d . . . C1 C 0.1219(4) 0.1381(3) 0.0625(2) 0.0516(11) Uani 1 1 d . . . C2 C 0.0293(4) 0.2019(3) 0.08393(18) 0.0419(10) Uani 1 1 d . . . C3 C -0.0873(4) 0.1973(3) 0.0596(2) 0.0502(11) Uani 1 1 d . . . H3 H -0.1080 0.1512 0.0304 0.060 Uiso 1 1 calc R . . C4 C -0.1813(3) 0.2534(3) 0.0727(2) 0.0481(11) Uani 1 1 d . . . C5 C -0.2748(3) 0.3750(3) 0.1132(2) 0.0532(12) Uani 1 1 d . . . H5A H -0.3305 0.3444 0.1400 0.064 Uiso 1 1 calc R . . H5B H -0.3150 0.3830 0.0679 0.064 Uiso 1 1 calc R . . C6 C -0.2492(3) 0.4603(3) 0.1437(2) 0.0514(12) Uani 1 1 d . . . H6A H -0.2067 0.4518 0.1883 0.062 Uiso 1 1 calc R . . H6B H -0.3257 0.4882 0.1504 0.062 Uiso 1 1 calc R . . C7 C -0.1767(3) 0.5203(3) 0.1048(2) 0.0456(11) Uani 1 1 d . . . H7A H -0.2059 0.5173 0.0571 0.055 Uiso 1 1 calc R . . H7B H -0.1886 0.5791 0.1202 0.055 Uiso 1 1 calc R . . C8 C 0.0196(3) 0.5515(2) 0.08083(18) 0.0371(9) Uani 1 1 d . . . C9 C 0.1465(3) 0.5443(2) 0.08413(18) 0.0378(9) Uani 1 1 d . . . H9 H 0.1856 0.5784 0.0539 0.045 Uiso 1 1 calc R . . C10 C 0.2169(3) 0.4940(3) 0.12576(19) 0.0372(9) Uani 1 1 d . . . C11 C 0.3526(3) 0.4904(3) 0.1251(2) 0.0422(10) Uani 1 1 d . . . C12 C 0.0915(5) 0.1042(3) -0.0083(2) 0.0820(17) Uani 1 1 d . . . H12A H 0.0796 0.1519 -0.0393 0.123 Uiso 1 1 calc R . . H12B H 0.0186 0.0703 -0.0096 0.123 Uiso 1 1 calc R . . H12C H 0.1568 0.0685 -0.0212 0.123 Uiso 1 1 calc R . . C13 C 0.1279(4) 0.0642(3) 0.1120(2) 0.0710(14) Uani 1 1 d . . . H13A H 0.0499 0.0368 0.1111 0.106 Uiso 1 1 calc R . . H13B H 0.1507 0.0857 0.1569 0.106 Uiso 1 1 calc R . . H13C H 0.1869 0.0228 0.0997 0.106 Uiso 1 1 calc R . . C14 C 0.2437(4) 0.1807(3) 0.0642(2) 0.0658(14) Uani 1 1 d . . . H14A H 0.2391 0.2299 0.0342 0.099 Uiso 1 1 calc R . . H14B H 0.3018 0.1400 0.0497 0.099 Uiso 1 1 calc R . . H14C H 0.2682 0.1994 0.1097 0.099 Uiso 1 1 calc R . . C15 C -0.3024(4) 0.2281(3) 0.0385(2) 0.0738(16) Uani 1 1 d . . . H15A H -0.3613 0.2272 0.0715 0.111 Uiso 1 1 calc R . . H15B H -0.2969 0.1715 0.0187 0.111 Uiso 1 1 calc R . . H15C H -0.3266 0.2694 0.0036 0.111 Uiso 1 1 calc R . . C16 C -0.0322(3) 0.6237(2) 0.0378(2) 0.0505(11) Uani 1 1 d . . . H16A H -0.0901 0.6010 0.0033 0.076 Uiso 1 1 calc R . . H16B H 0.0317 0.6526 0.0167 0.076 Uiso 1 1 calc R . . H16C H -0.0715 0.6643 0.0655 0.076 Uiso 1 1 calc R . . C17 C 0.4032(3) 0.5593(3) 0.0835(2) 0.0742(16) Uani 1 1 d . . . H17A H 0.3816 0.6151 0.1003 0.111 Uiso 1 1 calc R . . H17B H 0.3708 0.5533 0.0370 0.111 Uiso 1 1 calc R . . H17C H 0.4898 0.5541 0.0862 0.111 Uiso 1 1 calc R . . C18 C 0.3816(4) 0.4052(3) 0.0954(3) 0.0776(16) Uani 1 1 d . . . H18A H 0.3441 0.4014 0.0498 0.116 Uiso 1 1 calc R . . H18B H 0.3516 0.3595 0.1224 0.116 Uiso 1 1 calc R . . H18C H 0.4678 0.3996 0.0948 0.116 Uiso 1 1 calc R . . C19 C 0.4082(3) 0.4965(3) 0.1967(2) 0.0693(15) Uani 1 1 d . . . H19A H 0.3894 0.5519 0.2154 0.104 Uiso 1 1 calc R . . H19B H 0.4945 0.4903 0.1974 0.104 Uiso 1 1 calc R . . H19C H 0.3763 0.4513 0.2234 0.104 Uiso 1 1 calc R . . C21 C -0.1015(4) 0.2640(3) 0.4003(2) 0.0661(13) Uani 1 1 d . . . H21A H -0.1413 0.2109 0.4105 0.099 Uiso 1 1 calc R . . H21B H -0.1249 0.3090 0.4301 0.099 Uiso 1 1 calc R . . H21C H -0.0153 0.2560 0.4065 0.099 Uiso 1 1 calc R . . C22 C -0.1019(4) 0.2034(3) 0.2601(2) 0.0612(13) Uani 1 1 d . . . H22A H -0.1362 0.1509 0.2762 0.092 Uiso 1 1 calc R . . H22B H -0.0151 0.1985 0.2634 0.092 Uiso 1 1 calc R . . H22C H -0.1314 0.2128 0.2135 0.092 Uiso 1 1 calc R . . C23 C -0.3121(4) 0.2965(3) 0.3032(3) 0.0874(18) Uani 1 1 d . . . H23A H -0.3422 0.2456 0.3241 0.131 Uiso 1 1 calc R . . H23B H -0.3407 0.2976 0.2559 0.131 Uiso 1 1 calc R . . H23C H -0.3403 0.3473 0.3253 0.131 Uiso 1 1 calc R . . C31 C -0.0093(4) 0.4829(3) 0.4125(2) 0.0794(16) Uani 1 1 d . . . H31A H 0.0735 0.4649 0.4114 0.119 Uiso 1 1 calc R . . H31B H -0.0501 0.4442 0.4410 0.119 Uiso 1 1 calc R . . H31C H -0.0117 0.5408 0.4303 0.119 Uiso 1 1 calc R . . C32 C -0.2404(5) 0.5199(3) 0.3351(3) 0.0936(19) Uani 1 1 d . . . H32A H -0.2871 0.5171 0.2919 0.140 Uiso 1 1 calc R . . H32B H -0.2373 0.5789 0.3509 0.140 Uiso 1 1 calc R . . H32C H -0.2776 0.4843 0.3673 0.140 Uiso 1 1 calc R . . C33 C -0.0076(5) 0.5629(3) 0.2796(2) 0.0880(18) Uani 1 1 d . . . H33A H 0.0741 0.5446 0.2749 0.132 Uiso 1 1 calc R . . H33B H -0.0065 0.6167 0.3042 0.132 Uiso 1 1 calc R . . H33C H -0.0496 0.5707 0.2355 0.132 Uiso 1 1 calc R . . O1S O 0.1722(2) 0.30340(17) 0.26841(12) 0.0442(7) Uani 1 1 d . . . C1S C 0.2593(4) 0.2427(3) 0.2545(2) 0.0754(16) Uani 1 1 d . . . H1SA H 0.2883 0.2546 0.2105 0.090 Uiso 1 1 calc R . . H1SB H 0.2243 0.1850 0.2533 0.090 Uiso 1 1 calc R . . C2S C 0.3562(4) 0.2472(4) 0.3056(3) 0.0878(18) Uani 1 1 d . . . H2SA H 0.3683 0.1912 0.3276 0.105 Uiso 1 1 calc R . . H2SB H 0.4303 0.2631 0.2858 0.105 Uiso 1 1 calc R . . C3S C 0.3278(5) 0.3091(4) 0.3525(3) 0.116(3) Uani 1 1 d . . . H3SA H 0.3914 0.3524 0.3581 0.139 Uiso 1 1 calc R . . H3SB H 0.3196 0.2821 0.3962 0.139 Uiso 1 1 calc R . . C4S C 0.2147(4) 0.3492(3) 0.3272(2) 0.0700(15) Uani 1 1 d . . . H4SA H 0.1564 0.3458 0.3611 0.084 Uiso 1 1 calc R . . H4SB H 0.2274 0.4097 0.3165 0.084 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 Nd 0.02397(10) 0.04602(13) 0.02800(10) 0.00215(11) 0.00214(7) 0.00129(11) Si1 0.0404(6) 0.0495(7) 0.0411(7) 0.0098(6) 0.0088(5) -0.0007(6) Si2 0.0741(9) 0.0466(8) 0.0364(7) -0.0034(6) 0.0088(6) 0.0075(7) O1 0.0402(15) 0.062(2) 0.0443(17) -0.0144(15) -0.0022(13) 0.0035(14) O2 0.0254(14) 0.070(2) 0.062(2) 0.0282(17) -0.0013(13) -0.0025(14) N1 0.0279(17) 0.057(2) 0.0371(19) 0.0110(17) -0.0007(14) -0.0057(16) N2 0.0244(16) 0.044(2) 0.0384(19) -0.0003(15) 0.0022(14) 0.0052(15) N3 0.0328(16) 0.042(2) 0.0303(16) 0.0026(15) 0.0054(13) 0.0044(15) C1 0.077(3) 0.040(3) 0.038(2) 0.001(2) 0.007(2) 0.001(2) C2 0.057(3) 0.041(3) 0.028(2) 0.0050(19) 0.0040(19) -0.006(2) C3 0.064(3) 0.043(3) 0.041(2) 0.001(2) -0.003(2) -0.017(2) C4 0.041(2) 0.064(3) 0.038(2) 0.016(2) -0.0081(19) -0.022(2) C5 0.026(2) 0.083(3) 0.050(3) 0.019(3) -0.0022(18) -0.001(2) C6 0.023(2) 0.086(4) 0.046(3) 0.007(3) 0.0067(18) 0.017(2) C7 0.031(2) 0.062(3) 0.045(2) 0.008(2) 0.0031(18) 0.010(2) C8 0.039(2) 0.038(2) 0.034(2) -0.0004(18) -0.0016(18) 0.0054(19) C9 0.033(2) 0.042(2) 0.039(2) 0.0051(19) 0.0038(17) -0.0046(19) C10 0.030(2) 0.044(2) 0.038(2) -0.0043(19) 0.0041(17) -0.0042(18) C11 0.026(2) 0.056(3) 0.045(2) 0.003(2) 0.0050(18) -0.0067(19) C12 0.117(4) 0.080(4) 0.049(3) -0.018(3) 0.007(3) 0.016(3) C13 0.101(4) 0.049(3) 0.063(3) 0.006(3) 0.010(3) 0.006(3) C14 0.073(3) 0.055(3) 0.073(3) -0.008(3) 0.028(3) 0.012(3) C15 0.057(3) 0.083(4) 0.077(4) 0.008(3) -0.026(3) -0.024(3) C16 0.046(2) 0.051(3) 0.053(3) 0.011(2) 0.000(2) 0.006(2) C17 0.035(2) 0.103(4) 0.086(4) 0.035(3) 0.008(2) -0.010(3) C18 0.034(3) 0.083(4) 0.116(5) -0.017(3) 0.010(3) 0.007(3) C19 0.038(2) 0.119(4) 0.050(3) 0.004(3) -0.003(2) -0.014(3) C21 0.091(3) 0.058(3) 0.050(3) 0.013(2) 0.013(3) -0.007(3) C22 0.087(3) 0.042(3) 0.055(3) 0.005(2) 0.011(3) -0.011(3) C23 0.046(3) 0.097(4) 0.121(5) 0.031(4) 0.018(3) -0.006(3) C31 0.117(4) 0.072(4) 0.048(3) -0.016(3) 0.002(3) -0.002(3) C32 0.113(4) 0.082(4) 0.087(4) -0.012(3) 0.017(3) 0.051(4) C33 0.156(5) 0.052(3) 0.057(3) -0.014(3) 0.014(3) -0.031(4) O1S 0.0345(15) 0.0563(18) 0.0402(16) -0.0049(14) -0.0058(12) 0.0103(14) C1S 0.063(3) 0.084(4) 0.075(4) -0.023(3) -0.022(3) 0.030(3) C2S 0.064(3) 0.097(4) 0.096(5) -0.012(4) -0.029(3) 0.029(3) C3S 0.094(4) 0.151(6) 0.090(5) -0.051(4) -0.057(4) 0.067(4) C4S 0.061(3) 0.093(4) 0.052(3) -0.026(3) -0.014(2) 0.023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd O2 2.237(2) . ? Nd O1 2.265(3) . ? Nd N3 2.387(3) . ? Nd N1 2.549(3) . ? Nd N2 2.565(3) . ? Nd O1S 2.607(2) . ? Nd Si1 3.4461(11) . ? Si1 N3 1.700(3) . ? Si1 C22 1.869(4) . ? Si1 C21 1.873(4) . ? Si1 C23 1.877(4) . ? Si2 N3 1.696(3) . ? Si2 C33 1.859(5) . ? Si2 C31 1.872(4) . ? Si2 C32 1.887(5) . ? O1 C2 1.283(4) . ? O2 C10 1.293(4) . ? N1 C4 1.295(5) . ? N1 C5 1.481(5) . ? N2 C8 1.304(4) . ? N2 C7 1.480(4) . ? C1 C14 1.529(6) . ? C1 C13 1.531(5) . ? C1 C12 1.534(6) . ? C1 C2 1.538(5) . ? C2 C3 1.368(5) . ? C3 C4 1.425(6) . ? C4 C15 1.530(5) . ? C5 C6 1.495(6) . ? C6 C7 1.514(5) . ? C8 C9 1.435(5) . ? C8 C16 1.517(5) . ? C9 C10 1.358(5) . ? C10 C11 1.537(5) . ? C11 C17 1.512(5) . ? C11 C18 1.516(6) . ? C11 C19 1.527(5) . ? O1S C1S 1.417(5) . ? O1S C4S 1.434(4) . ? C1S C2S 1.438(6) . ? C2S C3S 1.414(7) . ? C3S C4S 1.476(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nd O1 92.54(10) . . ? O2 Nd N3 120.40(10) . . ? O1 Nd N3 133.38(10) . . ? O2 Nd N1 133.97(10) . . ? O1 Nd N1 72.32(10) . . ? N3 Nd N1 99.71(10) . . ? O2 Nd N2 71.83(9) . . ? O1 Nd N2 113.68(9) . . ? N3 Nd N2 107.87(9) . . ? N1 Nd N2 75.24(10) . . ? O2 Nd O1S 75.71(9) . . ? O1 Nd O1S 77.94(8) . . ? N3 Nd O1S 79.58(8) . . ? N1 Nd O1S 137.69(10) . . ? N2 Nd O1S 145.78(9) . . ? O2 Nd Si1 140.51(7) . . ? O1 Nd Si1 107.40(7) . . ? N3 Nd Si1 26.81(7) . . ? N1 Nd Si1 85.17(7) . . ? N2 Nd Si1 125.50(7) . . ? O1S Nd Si1 75.70(6) . . ? N3 Si1 C22 109.92(17) . . ? N3 Si1 C21 114.89(18) . . ? C22 Si1 C21 105.7(2) . . ? N3 Si1 C23 114.14(19) . . ? C22 Si1 C23 105.7(2) . . ? C21 Si1 C23 105.8(2) . . ? N3 Si1 Nd 39.28(10) . . ? C22 Si1 Nd 71.19(13) . . ? C21 Si1 Nd 133.42(15) . . ? C23 Si1 Nd 120.03(17) . . ? N3 Si2 C33 110.18(19) . . ? N3 Si2 C31 115.38(19) . . ? C33 Si2 C31 105.0(2) . . ? N3 Si2 C32 113.0(2) . . ? C33 Si2 C32 107.7(3) . . ? C31 Si2 C32 104.9(2) . . ? C2 O1 Nd 142.1(2) . . ? C10 O2 Nd 140.0(2) . . ? C4 N1 C5 116.8(3) . . ? C4 N1 Nd 129.6(3) . . ? C5 N1 Nd 113.1(2) . . ? C8 N2 C7 116.1(3) . . ? C8 N2 Nd 129.0(2) . . ? C7 N2 Nd 114.9(2) . . ? Si2 N3 Si1 124.89(18) . . ? Si2 N3 Nd 121.17(15) . . ? Si1 N3 Nd 113.91(15) . . ? C14 C1 C13 109.2(4) . . ? C14 C1 C12 107.6(4) . . ? C13 C1 C12 109.6(4) . . ? C14 C1 C2 110.0(3) . . ? C13 C1 C2 107.7(4) . . ? C12 C1 C2 112.7(4) . . ? O1 C2 C3 122.8(4) . . ? O1 C2 C1 115.7(3) . . ? C3 C2 C1 121.5(4) . . ? C2 C3 C4 127.8(4) . . ? N1 C4 C3 124.4(3) . . ? N1 C4 C15 121.5(4) . . ? C3 C4 C15 114.1(4) . . ? N1 C5 C6 113.9(3) . . ? C5 C6 C7 116.1(4) . . ? N2 C7 C6 113.1(3) . . ? N2 C8 C9 123.8(3) . . ? N2 C8 C16 121.3(3) . . ? C9 C8 C16 114.8(3) . . ? C10 C9 C8 127.1(4) . . ? O2 C10 C9 122.9(3) . . ? O2 C10 C11 113.9(3) . . ? C9 C10 C11 123.1(4) . . ? C17 C11 C18 108.1(4) . . ? C17 C11 C19 109.6(4) . . ? C18 C11 C19 110.1(4) . . ? C17 C11 C10 113.9(3) . . ? C18 C11 C10 106.6(3) . . ? C19 C11 C10 108.5(3) . . ? C1S O1S C4S 108.3(3) . . ? C1S O1S Nd 127.6(2) . . ? C4S O1S Nd 119.6(2) . . ? O1S C1S C2S 108.9(4) . . ? C3S C2S C1S 108.0(4) . . ? C2S C3S C4S 107.7(4) . . ? O1S C4S C3S 106.7(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Nd Si1 N3 50.42(19) . . . . ? O1 Nd Si1 N3 167.38(16) . . . . ? N1 Nd Si1 N3 -122.86(17) . . . . ? N2 Nd Si1 N3 -54.85(17) . . . . ? O1S Nd Si1 N3 95.19(16) . . . . ? O2 Nd Si1 C22 -119.63(19) . . . . ? O1 Nd Si1 C22 -2.67(17) . . . . ? N3 Nd Si1 C22 -170.1(2) . . . . ? N1 Nd Si1 C22 67.09(17) . . . . ? N2 Nd Si1 C22 135.10(17) . . . . ? O1S Nd Si1 C22 -74.86(16) . . . . ? O2 Nd Si1 C21 -25.6(2) . . . . ? O1 Nd Si1 C21 91.4(2) . . . . ? N3 Nd Si1 C21 -76.0(2) . . . . ? N1 Nd Si1 C21 161.1(2) . . . . ? N2 Nd Si1 C21 -130.9(2) . . . . ? O1S Nd Si1 C21 19.2(2) . . . . ? O2 Nd Si1 C23 142.7(2) . . . . ? O1 Nd Si1 C23 -100.4(2) . . . . ? N3 Nd Si1 C23 92.3(3) . . . . ? N1 Nd Si1 C23 -30.6(2) . . . . ? N2 Nd Si1 C23 37.4(2) . . . . ? O1S Nd Si1 C23 -172.5(2) . . . . ? O2 Nd O1 C2 -138.7(4) . . . . ? N3 Nd O1 C2 83.6(4) . . . . ? N1 Nd O1 C2 -3.0(4) . . . . ? N2 Nd O1 C2 -67.5(4) . . . . ? O1S Nd O1 C2 146.5(4) . . . . ? Si1 Nd O1 C2 75.8(4) . . . . ? O1 Nd O2 C10 86.6(4) . . . . ? N3 Nd O2 C10 -128.0(4) . . . . ? N1 Nd O2 C10 18.9(5) . . . . ? N2 Nd O2 C10 -27.5(4) . . . . ? O1S Nd O2 C10 163.5(4) . . . . ? Si1 Nd O2 C10 -151.8(4) . . . . ? O2 Nd N1 C4 86.0(4) . . . . ? O1 Nd N1 C4 10.0(3) . . . . ? N3 Nd N1 C4 -122.6(3) . . . . ? N2 Nd N1 C4 131.4(3) . . . . ? O1S Nd N1 C4 -37.4(4) . . . . ? Si1 Nd N1 C4 -100.0(3) . . . . ? O2 Nd N1 C5 -102.6(3) . . . . ? O1 Nd N1 C5 -178.6(3) . . . . ? N3 Nd N1 C5 48.8(2) . . . . ? N2 Nd N1 C5 -57.2(2) . . . . ? O1S Nd N1 C5 134.0(2) . . . . ? Si1 Nd N1 C5 71.4(2) . . . . ? O2 Nd N2 C8 13.2(3) . . . . ? O1 Nd N2 C8 -71.5(3) . . . . ? N3 Nd N2 C8 130.1(3) . . . . ? N1 Nd N2 C8 -134.2(3) . . . . ? O1S Nd N2 C8 32.3(4) . . . . ? Si1 Nd N2 C8 152.9(3) . . . . ? O2 Nd N2 C7 -166.1(3) . . . . ? O1 Nd N2 C7 109.2(2) . . . . ? N3 Nd N2 C7 -49.1(3) . . . . ? N1 Nd N2 C7 46.5(2) . . . . ? O1S Nd N2 C7 -147.0(2) . . . . ? Si1 Nd N2 C7 -26.3(3) . . . . ? C33 Si2 N3 Si1 -178.5(2) . . . . ? C31 Si2 N3 Si1 62.8(3) . . . . ? C32 Si2 N3 Si1 -58.0(3) . . . . ? C33 Si2 N3 Nd -0.8(3) . . . . ? C31 Si2 N3 Nd -119.5(2) . . . . ? C32 Si2 N3 Nd 119.7(2) . . . . ? C22 Si1 N3 Si2 -172.1(2) . . . . ? C21 Si1 N3 Si2 -53.1(3) . . . . ? C23 Si1 N3 Si2 69.3(3) . . . . ? Nd Si1 N3 Si2 177.9(3) . . . . ? C22 Si1 N3 Nd 10.0(2) . . . . ? C21 Si1 N3 Nd 129.01(19) . . . . ? C23 Si1 N3 Nd -108.6(2) . . . . ? O2 Nd N3 Si2 36.7(2) . . . . ? O1 Nd N3 Si2 165.39(13) . . . . ? N1 Nd N3 Si2 -119.82(17) . . . . ? N2 Nd N3 Si2 -42.32(18) . . . . ? O1S Nd N3 Si2 103.18(17) . . . . ? Si1 Nd N3 Si2 -177.9(3) . . . . ? O2 Nd N3 Si1 -145.37(13) . . . . ? O1 Nd N3 Si1 -16.7(2) . . . . ? N1 Nd N3 Si1 58.12(16) . . . . ? N2 Nd N3 Si1 135.62(14) . . . . ? O1S Nd N3 Si1 -78.88(14) . . . . ? Nd O1 C2 C3 -2.3(7) . . . . ? Nd O1 C2 C1 179.1(3) . . . . ? C14 C1 C2 O1 -31.9(5) . . . . ? C13 C1 C2 O1 87.1(4) . . . . ? C12 C1 C2 O1 -151.9(4) . . . . ? C14 C1 C2 C3 149.5(4) . . . . ? C13 C1 C2 C3 -91.5(4) . . . . ? C12 C1 C2 C3 29.5(6) . . . . ? O1 C2 C3 C4 4.2(7) . . . . ? C1 C2 C3 C4 -177.3(4) . . . . ? C5 N1 C4 C3 176.5(4) . . . . ? Nd N1 C4 C3 -12.4(6) . . . . ? C5 N1 C4 C15 -1.2(5) . . . . ? Nd N1 C4 C15 169.9(3) . . . . ? C2 C3 C4 N1 3.8(7) . . . . ? C2 C3 C4 C15 -178.4(4) . . . . ? C4 N1 C5 C6 -169.0(3) . . . . ? Nd N1 C5 C6 18.4(4) . . . . ? N1 C5 C6 C7 65.3(4) . . . . ? C8 N2 C7 C6 -178.2(3) . . . . ? Nd N2 C7 C6 1.2(4) . . . . ? C5 C6 C7 N2 -78.4(4) . . . . ? C7 N2 C8 C9 177.5(3) . . . . ? Nd N2 C8 C9 -1.8(5) . . . . ? C7 N2 C8 C16 -2.7(5) . . . . ? Nd N2 C8 C16 178.0(2) . . . . ? N2 C8 C9 C10 -10.3(6) . . . . ? C16 C8 C9 C10 169.9(4) . . . . ? Nd O2 C10 C9 26.9(7) . . . . ? Nd O2 C10 C11 -152.1(3) . . . . ? C8 C9 C10 O2 0.7(6) . . . . ? C8 C9 C10 C11 179.6(4) . . . . ? O2 C10 C11 C17 -170.1(4) . . . . ? C9 C10 C11 C17 11.0(6) . . . . ? O2 C10 C11 C18 70.8(5) . . . . ? C9 C10 C11 C18 -108.2(5) . . . . ? O2 C10 C11 C19 -47.8(5) . . . . ? C9 C10 C11 C19 133.3(4) . . . . ? O2 Nd O1S C1S -79.7(4) . . . . ? O1 Nd O1S C1S 16.1(3) . . . . ? N3 Nd O1S C1S 155.0(4) . . . . ? N1 Nd O1S C1S 62.0(4) . . . . ? N2 Nd O1S C1S -98.5(4) . . . . ? Si1 Nd O1S C1S 127.8(3) . . . . ? O2 Nd O1S C4S 73.5(3) . . . . ? O1 Nd O1S C4S 169.3(3) . . . . ? N3 Nd O1S C4S -51.8(3) . . . . ? N1 Nd O1S C4S -144.8(3) . . . . ? N2 Nd O1S C4S 54.7(4) . . . . ? Si1 Nd O1S C4S -79.0(3) . . . . ? C4S O1S C1S C2S 1.9(6) . . . . ? Nd O1S C1S C2S 157.6(3) . . . . ? O1S C1S C2S C3S 1.8(7) . . . . ? C1S C2S C3S C4S -4.7(8) . . . . ? C1S O1S C4S C3S -4.7(6) . . . . ? Nd O1S C4S C3S -162.6(4) . . . . ? C2S C3S C4S O1S 5.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 1.283 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.090 data_jbi4 _database_code_CSD 218982 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Bis-5,5’-(1,3-propanediyldiimino)-2,2-dimethyl-4-hexene-3-onato] lanthanum [bis(trimethylsilyl)-amido][tetrahydrofuran] ; _chemical_name_common ? _chemical_melting_point 120-123 _chemical_formula_moiety ? _chemical_formula_sum 'C29 H58 La N3 O3 Si2' _chemical_formula_weight 691.87 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3610(15) _cell_length_b 15.812(2) _cell_length_c 20.387(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.909(2) _cell_angle_gamma 90.00 _cell_volume 3648.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 3201 _cell_measurement_theta_min 2.213 _cell_measurement_theta_max 20.81 _exptl_crystal_description Rhombus _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 1.266 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4072 _exptl_absorpt_correction_T_max 0.4533 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD Area Detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 19926 _diffrn_reflns_av_R_equivalents 0.1097 _diffrn_reflns_av_sigmaI/netI 0.1541 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.34 _reflns_number_total 6646 _reflns_number_gt 3439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections except 2 which were flagged by the user for possible systematic errors. 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^)+(0.0229P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6646 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1345 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.0803 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _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 La La 0.01137(3) 0.37126(2) 0.187050(16) 0.03737(11) Uani 1 1 d . . . Si1 Si -0.14813(14) 0.29531(11) 0.31412(8) 0.0484(5) Uani 1 1 d . . . Si2 Si -0.08804(17) 0.48124(11) 0.32761(8) 0.0590(5) Uani 1 1 d . . . O1 O 0.0677(3) 0.2545(3) 0.12805(17) 0.0575(11) Uani 1 1 d . . . O2 O 0.1767(3) 0.4483(3) 0.16953(19) 0.0651(13) Uani 1 1 d . . . N1 N -0.1676(4) 0.3208(3) 0.1067(2) 0.0426(13) Uani 1 1 d . . . N2 N -0.0469(3) 0.5017(3) 0.1114(2) 0.0384(12) Uani 1 1 d . . . N3 N -0.0845(3) 0.3860(3) 0.28919(18) 0.0346(11) Uani 1 1 d . . . C1 C 0.1220(6) 0.1367(4) 0.0630(3) 0.0583(17) Uani 1 1 d . . . C2 C 0.0293(6) 0.1996(4) 0.0839(3) 0.0465(16) Uani 1 1 d . . . C3 C -0.0860(6) 0.1968(4) 0.0593(3) 0.0544(17) Uani 1 1 d . . . H3 H -0.1063 0.1515 0.0299 0.065 Uiso 1 1 calc R . . C4 C -0.1802(5) 0.2524(5) 0.0715(3) 0.0508(17) Uani 1 1 d . . . C5 C -0.2740(4) 0.3743(5) 0.1119(3) 0.0591(17) Uani 1 1 d . . . H5A H -0.3295 0.3436 0.1384 0.071 Uiso 1 1 calc R . . H5B H -0.3139 0.3826 0.0673 0.071 Uiso 1 1 calc R . . C6 C -0.2479(4) 0.4605(4) 0.1431(3) 0.0562(18) Uani 1 1 d . . . H6A H -0.2051 0.4517 0.1869 0.067 Uiso 1 1 calc R . . H6B H -0.3240 0.4881 0.1501 0.067 Uiso 1 1 calc R . . C7 C -0.1759(4) 0.5207(4) 0.1041(3) 0.0487(16) Uani 1 1 d . . . H7A H -0.2046 0.5174 0.0570 0.058 Uiso 1 1 calc R . . H7B H -0.1885 0.5793 0.1192 0.058 Uiso 1 1 calc R . . C8 C 0.0197(5) 0.5522(4) 0.0801(3) 0.0396(15) Uani 1 1 d . . . C9 C 0.1465(5) 0.5456(3) 0.0833(3) 0.0412(15) Uani 1 1 d . . . H9 H 0.1847 0.5787 0.0525 0.049 Uiso 1 1 calc R . . C10 C 0.2181(5) 0.4977(4) 0.1252(3) 0.0407(15) Uani 1 1 d . . . C11 C 0.3523(4) 0.4923(4) 0.1250(3) 0.0419(15) Uani 1 1 d . . . C12 C 0.0943(6) 0.1037(4) -0.0071(3) 0.089(2) Uani 1 1 d . . . H12A H 0.0878 0.1514 -0.0378 0.133 Uiso 1 1 calc R . . H12B H 0.0195 0.0725 -0.0098 0.133 Uiso 1 1 calc R . . H12C H 0.1579 0.0659 -0.0185 0.133 Uiso 1 1 calc R . . C13 C 0.1269(6) 0.0623(4) 0.1126(3) 0.085(2) Uani 1 1 d . . . H13A H 0.0504 0.0333 0.1098 0.128 Uiso 1 1 calc R . . H13B H 0.1450 0.0841 0.1574 0.128 Uiso 1 1 calc R . . H13C H 0.1886 0.0224 0.1021 0.128 Uiso 1 1 calc R . . C14 C 0.2439(5) 0.1802(4) 0.0652(3) 0.073(2) Uani 1 1 d . . . H14A H 0.2387 0.2302 0.0366 0.109 Uiso 1 1 calc R . . H14B H 0.3019 0.1406 0.0498 0.109 Uiso 1 1 calc R . . H14C H 0.2685 0.1974 0.1104 0.109 Uiso 1 1 calc R . . C15 C -0.3007(5) 0.2283(4) 0.0377(3) 0.073(2) Uani 1 1 d . . . H15A H -0.3589 0.2262 0.0705 0.110 Uiso 1 1 calc R . . H15B H -0.2954 0.1726 0.0170 0.110 Uiso 1 1 calc R . . H15C H -0.3250 0.2705 0.0041 0.110 Uiso 1 1 calc R . . C16 C -0.0310(4) 0.6234(3) 0.0365(2) 0.0520(15) Uani 1 1 d . . . H16A H -0.0870 0.6001 0.0019 0.078 Uiso 1 1 calc R . . H16B H 0.0331 0.6523 0.0163 0.078 Uiso 1 1 calc R . . H16C H -0.0720 0.6637 0.0630 0.078 Uiso 1 1 calc R . . C17 C 0.4028(5) 0.5587(4) 0.0814(3) 0.083(2) Uani 1 1 d . . . H17A H 0.3883 0.6151 0.0989 0.124 Uiso 1 1 calc R . . H17B H 0.3645 0.5540 0.0366 0.124 Uiso 1 1 calc R . . H17C H 0.4880 0.5498 0.0806 0.124 Uiso 1 1 calc R . . C18 C 0.3808(5) 0.4047(4) 0.0975(4) 0.090(3) Uani 1 1 d . . . H18A H 0.3436 0.3991 0.0525 0.135 Uiso 1 1 calc R . . H18B H 0.3502 0.3606 0.1253 0.135 Uiso 1 1 calc R . . H18C H 0.4665 0.3984 0.0972 0.135 Uiso 1 1 calc R . . C19 C 0.4087(5) 0.5000(4) 0.1943(3) 0.077(2) Uani 1 1 d . . . H19A H 0.3879 0.5548 0.2127 0.116 Uiso 1 1 calc R . . H19B H 0.4948 0.4960 0.1941 0.116 Uiso 1 1 calc R . . H19C H 0.3802 0.4544 0.2214 0.116 Uiso 1 1 calc R . . C21 C -0.1031(5) 0.2623(4) 0.4010(3) 0.072(2) Uani 1 1 d . . . H21A H -0.1421 0.2090 0.4104 0.108 Uiso 1 1 calc R . . H21B H -0.1263 0.3061 0.4313 0.108 Uiso 1 1 calc R . . H21C H -0.0172 0.2546 0.4066 0.108 Uiso 1 1 calc R . . C22 C -0.1052(5) 0.2044(3) 0.2615(3) 0.071(2) Uani 1 1 d . . . H22A H -0.1389 0.1518 0.2772 0.106 Uiso 1 1 calc R . . H22B H -0.0189 0.1996 0.2642 0.106 Uiso 1 1 calc R . . H22C H -0.1355 0.2143 0.2157 0.106 Uiso 1 1 calc R . . C23 C -0.3138(5) 0.2969(4) 0.3059(3) 0.094(3) Uani 1 1 d . . . H23A H -0.3438 0.2421 0.3196 0.142 Uiso 1 1 calc R . . H23B H -0.3421 0.3077 0.2599 0.142 Uiso 1 1 calc R . . H23C H -0.3420 0.3416 0.3338 0.142 Uiso 1 1 calc R . . C31 C -0.0133(6) 0.4836(4) 0.4131(3) 0.087(2) Uani 1 1 d . . . H31A H 0.0673 0.4618 0.4127 0.130 Uiso 1 1 calc R . . H31B H -0.0576 0.4484 0.4420 0.130 Uiso 1 1 calc R . . H31C H -0.0107 0.5420 0.4295 0.130 Uiso 1 1 calc R . . C32 C -0.2427(6) 0.5219(4) 0.3352(3) 0.101(3) Uani 1 1 d . . . H32A H -0.2864 0.5227 0.2916 0.151 Uiso 1 1 calc R . . H32B H -0.2387 0.5793 0.3533 0.151 Uiso 1 1 calc R . . H32C H -0.2831 0.4848 0.3645 0.151 Uiso 1 1 calc R . . C33 C -0.0114(6) 0.5626(4) 0.2810(3) 0.095(3) Uani 1 1 d . . . H33A H 0.0692 0.5438 0.2752 0.143 Uiso 1 1 calc R . . H33B H -0.0086 0.6161 0.3054 0.143 Uiso 1 1 calc R . . H33C H -0.0545 0.5710 0.2377 0.143 Uiso 1 1 calc R . . O1S O 0.1773(3) 0.3021(2) 0.27036(17) 0.0469(10) Uani 1 1 d . . . C1S C 0.2644(6) 0.2420(5) 0.2573(3) 0.087(2) Uani 1 1 d . . . H1SA H 0.2931 0.2534 0.2137 0.105 Uiso 1 1 calc R . . H1SB H 0.2297 0.1845 0.2564 0.105 Uiso 1 1 calc R . . C2S C 0.3607(6) 0.2461(5) 0.3068(4) 0.092(2) Uani 1 1 d . . . H2SA H 0.4341 0.2620 0.2870 0.110 Uiso 1 1 calc R . . H2SB H 0.3729 0.1904 0.3285 0.110 Uiso 1 1 calc R . . C3S C 0.3320(7) 0.3083(6) 0.3535(4) 0.127(4) Uani 1 1 d . . . H3SA H 0.3949 0.3517 0.3587 0.153 Uiso 1 1 calc R . . H3SB H 0.3246 0.2817 0.3969 0.153 Uiso 1 1 calc R . . C4S C 0.2187(5) 0.3476(4) 0.3289(3) 0.084(2) Uani 1 1 d . . . H4SA H 0.1608 0.3434 0.3624 0.101 Uiso 1 1 calc R . . H4SB H 0.2305 0.4081 0.3187 0.101 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 La 0.02856(17) 0.0535(2) 0.02998(18) 0.0022(2) 0.00217(12) 0.0020(2) Si1 0.0432(11) 0.0548(13) 0.0482(12) 0.0115(9) 0.0100(8) -0.0010(9) Si2 0.0854(15) 0.0520(13) 0.0397(12) -0.0030(10) 0.0072(10) 0.0061(11) O1 0.044(3) 0.080(3) 0.047(3) -0.020(2) -0.006(2) 0.007(2) O2 0.033(2) 0.094(4) 0.067(3) 0.037(3) -0.003(2) -0.003(2) N1 0.035(3) 0.054(4) 0.038(3) 0.010(3) -0.001(2) -0.007(3) N2 0.024(3) 0.055(3) 0.036(3) 0.002(2) 0.001(2) 0.003(2) N3 0.042(3) 0.035(3) 0.027(2) -0.001(2) 0.0052(19) 0.004(2) C1 0.088(5) 0.044(4) 0.043(4) -0.007(4) 0.007(3) 0.010(5) C2 0.063(5) 0.040(4) 0.036(4) 0.002(3) 0.003(3) -0.011(4) C3 0.067(5) 0.048(5) 0.045(4) 0.005(3) -0.012(4) -0.018(4) C4 0.046(5) 0.060(5) 0.044(4) 0.019(4) -0.013(3) -0.022(4) C5 0.030(3) 0.099(5) 0.046(4) 0.020(4) -0.008(3) 0.003(4) C6 0.026(3) 0.099(6) 0.044(4) 0.007(4) 0.009(3) 0.018(4) C7 0.035(4) 0.071(5) 0.040(4) 0.010(3) 0.000(3) 0.006(3) C8 0.039(4) 0.046(4) 0.033(4) -0.005(3) -0.002(3) 0.007(3) C9 0.039(4) 0.050(4) 0.035(4) 0.008(3) 0.002(3) -0.001(3) C10 0.031(4) 0.049(4) 0.043(4) -0.008(3) 0.008(3) -0.008(3) C11 0.028(3) 0.050(4) 0.048(4) 0.005(3) 0.005(3) -0.002(3) C12 0.128(6) 0.081(6) 0.057(5) -0.024(4) 0.000(4) 0.018(5) C13 0.128(7) 0.066(5) 0.063(5) 0.014(4) 0.012(4) 0.008(5) C14 0.080(5) 0.066(5) 0.076(5) -0.017(4) 0.025(4) 0.009(4) C15 0.063(5) 0.071(5) 0.080(5) 0.011(4) -0.030(4) -0.023(4) C16 0.049(4) 0.057(4) 0.048(4) 0.009(4) -0.002(3) 0.009(4) C17 0.038(4) 0.114(6) 0.097(6) 0.042(5) 0.008(4) -0.007(4) C18 0.036(4) 0.081(6) 0.154(7) -0.020(5) 0.016(4) 0.011(4) C19 0.039(4) 0.134(7) 0.058(5) -0.002(5) 0.002(3) -0.017(4) C21 0.112(6) 0.061(5) 0.044(4) 0.007(3) 0.012(4) -0.002(4) C22 0.101(6) 0.044(4) 0.066(5) 0.005(4) 0.005(4) -0.020(4) C23 0.053(5) 0.110(7) 0.123(7) 0.034(5) 0.019(4) -0.009(4) C31 0.129(7) 0.088(6) 0.043(4) -0.016(4) 0.003(4) 0.006(5) C32 0.114(6) 0.096(6) 0.093(6) -0.014(5) 0.011(5) 0.057(5) C33 0.153(7) 0.060(5) 0.071(5) -0.016(4) 0.002(5) -0.027(5) O1S 0.038(2) 0.060(3) 0.040(3) -0.010(2) -0.0124(19) 0.010(2) C1S 0.085(6) 0.088(6) 0.084(6) -0.029(4) -0.022(5) 0.045(5) C2S 0.068(5) 0.099(7) 0.100(7) -0.011(5) -0.037(5) 0.015(5) C3S 0.109(7) 0.175(9) 0.086(6) -0.048(6) -0.063(5) 0.070(7) C4S 0.072(5) 0.117(7) 0.060(5) -0.026(5) -0.024(4) 0.033(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La O2 2.292(4) . ? La O1 2.323(4) . ? La N3 2.443(3) . ? La N1 2.624(5) . ? La N2 2.626(4) . ? La O1S 2.662(3) . ? La Si1 3.4986(16) . ? Si1 N3 1.703(4) . ? Si1 C21 1.875(5) . ? Si1 C23 1.875(6) . ? Si1 C22 1.883(5) . ? Si2 N3 1.699(4) . ? Si2 C33 1.861(6) . ? Si2 C31 1.873(6) . ? Si2 C32 1.889(6) . ? O1 C2 1.299(6) . ? O2 C10 1.312(6) . ? N1 C4 1.299(7) . ? N1 C5 1.486(6) . ? N2 C8 1.304(6) . ? N2 C7 1.491(5) . ? C1 C12 1.528(7) . ? C1 C2 1.534(7) . ? C1 C14 1.543(7) . ? C1 C13 1.550(7) . ? C2 C3 1.363(7) . ? C3 C4 1.422(8) . ? C4 C15 1.527(7) . ? C5 C6 1.522(7) . ? C6 C7 1.523(7) . ? C8 C9 1.440(6) . ? C8 C16 1.517(7) . ? C9 C10 1.358(7) . ? C10 C11 1.528(6) . ? C11 C19 1.507(7) . ? C11 C17 1.519(7) . ? C11 C18 1.539(7) . ? O1S C1S 1.414(6) . ? O1S C4S 1.439(6) . ? C1S C2S 1.424(8) . ? C2S C3S 1.428(8) . ? C3S C4S 1.477(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La O1 94.34(14) . . ? O2 La N3 120.88(14) . . ? O1 La N3 132.86(13) . . ? O2 La N1 131.73(13) . . ? O1 La N1 70.62(14) . . ? N3 La N1 100.56(13) . . ? O2 La N2 70.12(13) . . ? O1 La N2 112.75(13) . . ? N3 La N2 108.50(12) . . ? N1 La N2 74.27(14) . . ? O2 La O1S 76.87(12) . . ? O1 La O1S 78.02(12) . . ? N3 La O1S 80.70(12) . . ? N1 La O1S 137.91(13) . . ? N2 La O1S 145.76(12) . . ? O2 La Si1 141.35(10) . . ? O1 La Si1 107.08(10) . . ? N3 La Si1 26.43(10) . . ? N1 La Si1 86.30(9) . . ? N2 La Si1 125.74(9) . . ? O1S La Si1 76.69(8) . . ? N3 Si1 C21 115.3(2) . . ? N3 Si1 C23 114.2(2) . . ? C21 Si1 C23 106.2(3) . . ? N3 Si1 C22 109.6(2) . . ? C21 Si1 C22 105.2(3) . . ? C23 Si1 C22 105.4(3) . . ? N3 Si1 La 39.66(12) . . ? C21 Si1 La 132.7(2) . . ? C23 Si1 La 120.6(2) . . ? C22 Si1 La 70.39(17) . . ? N3 Si2 C33 110.3(2) . . ? N3 Si2 C31 114.9(3) . . ? C33 Si2 C31 105.5(3) . . ? N3 Si2 C32 113.4(3) . . ? C33 Si2 C32 106.6(3) . . ? C31 Si2 C32 105.5(3) . . ? C2 O1 La 143.0(4) . . ? C10 O2 La 140.4(3) . . ? C4 N1 C5 117.5(5) . . ? C4 N1 La 129.8(4) . . ? C5 N1 La 111.9(4) . . ? C8 N2 C7 115.8(4) . . ? C8 N2 La 129.8(3) . . ? C7 N2 La 114.4(3) . . ? Si2 N3 Si1 125.6(2) . . ? Si2 N3 La 120.5(2) . . ? Si1 N3 La 113.91(19) . . ? C12 C1 C2 112.9(5) . . ? C12 C1 C14 106.9(5) . . ? C2 C1 C14 109.8(5) . . ? C12 C1 C13 110.1(5) . . ? C2 C1 C13 107.4(5) . . ? C14 C1 C13 109.7(5) . . ? O1 C2 C3 122.1(6) . . ? O1 C2 C1 115.3(6) . . ? C3 C2 C1 122.6(6) . . ? C2 C3 C4 129.0(6) . . ? N1 C4 C3 124.2(6) . . ? N1 C4 C15 120.6(6) . . ? C3 C4 C15 115.2(6) . . ? N1 C5 C6 114.1(5) . . ? C5 C6 C7 115.9(5) . . ? N2 C7 C6 112.9(4) . . ? N2 C8 C9 123.6(5) . . ? N2 C8 C16 122.2(5) . . ? C9 C8 C16 114.1(5) . . ? C10 C9 C8 127.7(5) . . ? O2 C10 C9 122.4(5) . . ? O2 C10 C11 112.7(5) . . ? C9 C10 C11 125.0(5) . . ? C19 C11 C17 109.9(5) . . ? C19 C11 C10 109.7(4) . . ? C17 C11 C10 112.9(5) . . ? C19 C11 C18 109.2(5) . . ? C17 C11 C18 108.0(5) . . ? C10 C11 C18 107.0(4) . . ? C1S O1S C4S 107.9(4) . . ? C1S O1S La 128.7(3) . . ? C4S O1S La 119.2(3) . . ? O1S C1S C2S 110.1(6) . . ? C1S C2S C3S 107.4(6) . . ? C2S C3S C4S 107.7(6) . . ? O1S C4S C3S 106.6(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 La Si1 N3 48.0(3) . . . . ? O1 La Si1 N3 168.7(2) . . . . ? N1 La Si1 N3 -122.9(2) . . . . ? N2 La Si1 N3 -55.3(2) . . . . ? O1S La Si1 N3 95.9(2) . . . . ? O2 La Si1 C21 -30.4(3) . . . . ? O1 La Si1 C21 90.3(3) . . . . ? N3 La Si1 C21 -78.4(3) . . . . ? N1 La Si1 C21 158.7(3) . . . . ? N2 La Si1 C21 -133.7(3) . . . . ? O1S La Si1 C21 17.5(3) . . . . ? O2 La Si1 C23 139.9(3) . . . . ? O1 La Si1 C23 -99.3(3) . . . . ? N3 La Si1 C23 92.0(3) . . . . ? N1 La Si1 C23 -30.9(3) . . . . ? N2 La Si1 C23 36.7(3) . . . . ? O1S La Si1 C23 -172.1(3) . . . . ? O2 La Si1 C22 -123.3(3) . . . . ? O1 La Si1 C22 -2.6(2) . . . . ? N3 La Si1 C22 -171.3(3) . . . . ? N1 La Si1 C22 65.8(2) . . . . ? N2 La Si1 C22 133.4(2) . . . . ? O1S La Si1 C22 -75.4(2) . . . . ? O2 La O1 C2 -134.1(6) . . . . ? N3 La O1 C2 85.3(6) . . . . ? N1 La O1 C2 -1.2(6) . . . . ? N2 La O1 C2 -63.9(6) . . . . ? O1S La O1 C2 150.3(6) . . . . ? Si1 La O1 C2 78.4(6) . . . . ? O1 La O2 C10 83.4(6) . . . . ? N3 La O2 C10 -129.4(6) . . . . ? N1 La O2 C10 15.7(7) . . . . ? N2 La O2 C10 -29.2(5) . . . . ? O1S La O2 C10 160.0(6) . . . . ? Si1 La O2 C10 -152.1(5) . . . . ? O2 La N1 C4 88.3(5) . . . . ? O1 La N1 C4 10.2(5) . . . . ? N3 La N1 C4 -121.7(5) . . . . ? N2 La N1 C4 131.8(5) . . . . ? O1S La N1 C4 -33.9(6) . . . . ? Si1 La N1 C4 -99.4(5) . . . . ? O2 La N1 C5 -101.9(4) . . . . ? O1 La N1 C5 180.0(4) . . . . ? N3 La N1 C5 48.1(3) . . . . ? N2 La N1 C5 -58.4(3) . . . . ? O1S La N1 C5 135.8(3) . . . . ? Si1 La N1 C5 70.4(3) . . . . ? O2 La N2 C8 13.7(4) . . . . ? O1 La N2 C8 -72.6(5) . . . . ? N3 La N2 C8 130.7(4) . . . . ? N1 La N2 C8 -133.2(5) . . . . ? O1S La N2 C8 29.8(6) . . . . ? Si1 La N2 C8 153.4(4) . . . . ? O2 La N2 C7 -165.5(4) . . . . ? O1 La N2 C7 108.1(3) . . . . ? N3 La N2 C7 -48.5(3) . . . . ? N1 La N2 C7 47.6(3) . . . . ? O1S La N2 C7 -149.4(3) . . . . ? Si1 La N2 C7 -25.8(4) . . . . ? C33 Si2 N3 Si1 -178.0(3) . . . . ? C31 Si2 N3 Si1 63.0(4) . . . . ? C32 Si2 N3 Si1 -58.5(4) . . . . ? C33 Si2 N3 La -0.2(3) . . . . ? C31 Si2 N3 La -119.3(3) . . . . ? C32 Si2 N3 La 119.2(3) . . . . ? C21 Si1 N3 Si2 -54.9(4) . . . . ? C23 Si1 N3 Si2 68.5(4) . . . . ? C22 Si1 N3 Si2 -173.5(3) . . . . ? La Si1 N3 Si2 177.9(4) . . . . ? C21 Si1 N3 La 127.2(2) . . . . ? C23 Si1 N3 La -109.3(3) . . . . ? C22 Si1 N3 La 8.7(3) . . . . ? O2 La N3 Si2 34.7(3) . . . . ? O1 La N3 Si2 167.23(19) . . . . ? N1 La N3 Si2 -119.5(2) . . . . ? N2 La N3 Si2 -42.7(3) . . . . ? O1S La N3 Si2 103.3(2) . . . . ? Si1 La N3 Si2 -178.0(4) . . . . ? O2 La N3 Si1 -147.28(18) . . . . ? O1 La N3 Si1 -14.8(3) . . . . ? N1 La N3 Si1 58.5(2) . . . . ? N2 La N3 Si1 135.29(19) . . . . ? O1S La N3 Si1 -78.8(2) . . . . ? La O1 C2 C3 -4.8(10) . . . . ? La O1 C2 C1 176.9(4) . . . . ? C12 C1 C2 O1 -152.7(5) . . . . ? C14 C1 C2 O1 -33.5(7) . . . . ? C13 C1 C2 O1 85.8(6) . . . . ? C12 C1 C2 C3 29.0(8) . . . . ? C14 C1 C2 C3 148.3(5) . . . . ? C13 C1 C2 C3 -92.5(7) . . . . ? O1 C2 C3 C4 5.0(10) . . . . ? C1 C2 C3 C4 -176.9(5) . . . . ? C5 N1 C4 C3 177.1(5) . . . . ? La N1 C4 C3 -13.6(8) . . . . ? C5 N1 C4 C15 -0.6(8) . . . . ? La N1 C4 C15 168.7(3) . . . . ? C2 C3 C4 N1 4.7(10) . . . . ? C2 C3 C4 C15 -177.5(5) . . . . ? C4 N1 C5 C6 -169.4(5) . . . . ? La N1 C5 C6 19.5(5) . . . . ? N1 C5 C6 C7 65.7(6) . . . . ? C8 N2 C7 C6 -178.8(5) . . . . ? La N2 C7 C6 0.5(6) . . . . ? C5 C6 C7 N2 -79.2(6) . . . . ? C7 N2 C8 C9 177.6(5) . . . . ? La N2 C8 C9 -1.7(8) . . . . ? C7 N2 C8 C16 -2.8(7) . . . . ? La N2 C8 C16 178.0(3) . . . . ? N2 C8 C9 C10 -11.2(9) . . . . ? C16 C8 C9 C10 169.1(5) . . . . ? La O2 C10 C9 28.8(9) . . . . ? La O2 C10 C11 -149.2(4) . . . . ? C8 C9 C10 O2 0.9(9) . . . . ? C8 C9 C10 C11 178.7(5) . . . . ? O2 C10 C11 C19 -48.2(7) . . . . ? C9 C10 C11 C19 133.9(6) . . . . ? O2 C10 C11 C17 -171.2(5) . . . . ? C9 C10 C11 C17 10.9(8) . . . . ? O2 C10 C11 C18 70.2(6) . . . . ? C9 C10 C11 C18 -107.8(6) . . . . ? O2 La O1S C1S -80.4(5) . . . . ? O1 La O1S C1S 17.0(5) . . . . ? N3 La O1S C1S 154.7(5) . . . . ? N1 La O1S C1S 59.2(5) . . . . ? N2 La O1S C1S -96.0(5) . . . . ? Si1 La O1S C1S 128.0(5) . . . . ? O2 La O1S C4S 73.6(4) . . . . ? O1 La O1S C4S 171.0(4) . . . . ? N3 La O1S C4S -51.3(4) . . . . ? N1 La O1S C4S -146.8(4) . . . . ? N2 La O1S C4S 58.0(5) . . . . ? Si1 La O1S C4S -78.0(4) . . . . ? C4S O1S C1S C2S 1.2(8) . . . . ? La O1S C1S C2S 157.5(5) . . . . ? O1S C1S C2S C3S 2.0(9) . . . . ? C1S C2S C3S C4S -4.3(10) . . . . ? C1S O1S C4S C3S -3.8(8) . . . . ? La O1S C4S C3S -162.7(5) . . . . ? C2S C3S C4S O1S 5.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.631 _refine_diff_density_min -0.386 _refine_diff_density_rms 0.091