# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jean-Francois Carpentier' _publ_contact_author_email JEAN-FRANCOIS.CARPENTIER@UNIV-RENNES1.FR _publ_section_title ; Group 3 Metal Complexes Supported by Tridentate Pyridine- and Thiophene-Linked Bis(naphtholate) Ligands: Synthesis, Structure, and Use in Stereoselective Ring-Opening Polymerization of Racemic Lactide and beta-Butyrolactone ; loop_ _publ_author_name 'Jean-Francois Carpentier' 'Ekaterina Grunova' 'Evgueni Kirillov' 'Thierry Roisnel' # Attachment 'Cif_files_B920283H.cif' data_complex3 _database_code_depnum_ccdc_archive 'CCDC 752787' #TrackingRef 'Cif_files_B920283H.cif' _audit_creation_date 2009-11-16T15:03:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C69 H65 La N2 O3 Si4' _chemical_formula_sum 'C69 H65 La N2 O3 Si4' _chemical_formula_weight 1221.5 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5427(13) _cell_length_b 13.2146(15) _cell_length_c 21.900(3) _cell_angle_alpha 72.485(6) _cell_angle_beta 83.460(6) _cell_angle_gamma 76.123(7) _cell_volume 3089.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2432 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 21.42 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.816 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.774 _exptl_absorpt_correction_T_max 0.968 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.12 _diffrn_reflns_av_unetI/netI 0.1853 _diffrn_reflns_number 32706 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 14021 _reflns_number_gt 9954 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART, 2006' _computing_cell_refinement 'Bruker SMART, 2006' _computing_data_reduction 'Bruker SAINT, 2006' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0641P)^2^+27.2696P] 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_number_reflns 14021 _refine_ls_number_parameters 702 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1753 _refine_ls_R_factor_gt 0.1307 _refine_ls_wR_factor_ref 0.2678 _refine_ls_wR_factor_gt 0.2464 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.201 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.444 _refine_diff_density_min -4.305 _refine_diff_density_rms 0.184 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.46065(6) 0.43833(5) 0.26434(3) 0.01550(16) Uani 1 1 d . A . O1 O 0.3875(6) 0.5513(6) 0.1653(4) 0.0248(17) Uani 1 1 d . . . O2 O 0.5385(6) 0.2614(6) 0.2619(3) 0.0248(17) Uani 1 1 d . A . N1 N 0.2853(8) 0.3557(7) 0.2480(4) 0.0229(19) Uani 1 1 d . A . C1 C 0.1851(9) 0.5507(8) 0.2015(5) 0.021(2) Uani 1 1 d . A . C2 C 0.2741(10) 0.6052(8) 0.1711(5) 0.025(2) Uani 1 1 d . . . C3 C 0.2420(9) 0.7241(8) 0.1434(5) 0.022(2) Uani 1 1 d . A . Si1 Si 0.3479(3) 0.8075(2) 0.09265(14) 0.0207(6) Uani 1 1 d . . . C4 C 0.1289(10) 0.7764(9) 0.1577(5) 0.025(2) Uani 1 1 d . . . H4 H 0.1078 0.8531 0.1403 0.03 Uiso 1 1 calc R A . C5 C -0.0691(10) 0.7805(9) 0.2151(6) 0.028(3) Uani 1 1 d . . . H5 H -0.0869 0.8577 0.2008 0.034 Uiso 1 1 calc R A . C6 C -0.1527(9) 0.7296(8) 0.2525(5) 0.024(2) Uani 1 1 d . A . H6 H -0.2275 0.7704 0.2634 0.029 Uiso 1 1 calc R . . C7 C -0.1258(11) 0.6152(9) 0.2748(6) 0.036(3) Uani 1 1 d . . . H7 H -0.1826 0.5785 0.3016 0.043 Uiso 1 1 calc R A . C8 C -0.0173(10) 0.5558(9) 0.2578(6) 0.031(3) Uani 1 1 d . A . H8 H -0.0007 0.4786 0.2728 0.037 Uiso 1 1 calc R . . C9 C 0.0695(10) 0.6090(8) 0.2183(5) 0.025(2) Uani 1 1 d . . . C10 C 0.0416(10) 0.7245(8) 0.1966(5) 0.024(2) Uani 1 1 d . A . C11 C 0.1999(9) 0.4314(8) 0.2103(5) 0.024(2) Uani 1 1 d . . . C12 C 0.1254(10) 0.3986(9) 0.1781(6) 0.031(3) Uani 1 1 d . A . H12 H 0.0633 0.4513 0.154 0.038 Uiso 1 1 calc R . . C13 C 0.1399(11) 0.2908(9) 0.1805(6) 0.035(3) Uani 1 1 d . . . H13 H 0.0913 0.2687 0.1569 0.041 Uiso 1 1 calc R A . C14 C 0.2280(9) 0.2157(9) 0.2187(5) 0.026(2) Uani 1 1 d . A . H14 H 0.2417 0.141 0.2205 0.031 Uiso 1 1 calc R . . C15 C 0.2964(9) 0.2491(8) 0.2543(5) 0.022(2) Uani 1 1 d . . . C21 C 0.3823(9) 0.1658(7) 0.2995(5) 0.020(2) Uani 1 1 d . A . C22 C 0.5011(9) 0.1737(8) 0.2991(5) 0.021(2) Uani 1 1 d . . . C23 C 0.5870(9) 0.0871(8) 0.3370(5) 0.019(2) Uani 1 1 d . A . Si2 Si 0.7489(3) 0.0949(2) 0.33225(14) 0.0217(6) Uani 1 1 d . . . C24 C 0.5470(9) 0.0020(8) 0.3783(5) 0.023(2) Uani 1 1 d . . . H24 H 0.6035 -0.0547 0.4043 0.027 Uiso 1 1 calc R A . C25 C 0.3881(10) -0.0976(9) 0.4300(5) 0.027(2) Uani 1 1 d . . . H25 H 0.4444 -0.1515 0.4575 0.032 Uiso 1 1 calc R A . C26 C 0.2724(11) -0.1084(9) 0.4346(6) 0.032(3) Uani 1 1 d . A . H26 H 0.2495 -0.171 0.4632 0.039 Uiso 1 1 calc R . . C27 C 0.1876(10) -0.0257(9) 0.3964(5) 0.027(2) Uani 1 1 d . . . H27 H 0.1065 -0.0317 0.4002 0.032 Uiso 1 1 calc R A . C28 C 0.2207(9) 0.0641(9) 0.3534(6) 0.027(2) Uani 1 1 d . A . H28 H 0.1613 0.1199 0.329 0.032 Uiso 1 1 calc R . . C29 C 0.3413(10) 0.0755(8) 0.3445(5) 0.022(2) Uani 1 1 d . . . C30 C 0.4262(9) -0.0078(8) 0.3851(5) 0.021(2) Uani 1 1 d . A . O3 O 0.6606(7) 0.4885(6) 0.2232(4) 0.035(2) Uani 1 1 d . . . C31 C 0.6614(12) 0.5982(10) 0.1821(7) 0.047(4) Uani 1 1 d . . . H31A H 0.678 0.6443 0.2069 0.056 Uiso 1 1 calc R . . H31B H 0.5839 0.6327 0.1617 0.056 Uiso 1 1 calc R . . C32 C 0.7616(13) 0.5812(12) 0.1321(7) 0.054(4) Uani 1 1 d . . . H32A H 0.7376 0.6276 0.0888 0.065 Uiso 1 1 calc R . . H32B H 0.8349 0.5984 0.1421 0.065 Uiso 1 1 calc R . . C33 C 0.7823(13) 0.4614(11) 0.1358(7) 0.047(3) Uani 1 1 d . . . H33A H 0.7258 0.4486 0.1097 0.056 Uiso 1 1 calc R . . H33B H 0.8652 0.4329 0.1218 0.056 Uiso 1 1 calc R . . C34 C 0.7597(11) 0.4134(10) 0.2041(6) 0.041(3) Uani 1 1 d . . . H34A H 0.7397 0.3417 0.2119 0.05 Uiso 1 1 calc R . . H34B H 0.8308 0.4039 0.2283 0.05 Uiso 1 1 calc R . . C41 C 0.2550(9) 0.9443(9) 0.0497(5) 0.024(2) Uani 1 1 d . A . C42 C 0.1755(9) 0.9525(9) 0.0048(5) 0.024(2) Uani 1 1 d . . . H42 H 0.1581 0.8879 0.001 0.029 Uiso 1 1 calc R A . C43 C 0.1203(11) 1.0524(10) -0.0353(6) 0.033(3) Uani 1 1 d . A . H43 H 0.0659 1.0553 -0.0655 0.04 Uiso 1 1 calc R . . C44 C 0.1450(12) 1.1477(10) -0.0307(6) 0.037(3) Uani 1 1 d . . . H44 H 0.1087 1.216 -0.0583 0.044 Uiso 1 1 calc R A . C45 C 0.2229(13) 1.1423(10) 0.0142(7) 0.043(3) Uani 1 1 d . A . H45 H 0.24 1.2069 0.018 0.052 Uiso 1 1 calc R . . C46 C 0.2769(10) 1.0400(9) 0.0546(6) 0.032(3) Uani 1 1 d . . . H46 H 0.3295 1.0369 0.0858 0.038 Uiso 1 1 calc R A . C47A C 0.4345(11) 0.7565(10) 0.0242(6) 0.0342(16) Uani 0.590(13) 1 d P A 1 C48A C 0.467(4) 0.834(3) -0.031(2) 0.0342(16) Uani 0.590(13) 1 d P A 1 H48A H 0.4532 0.9085 -0.033 0.041 Uiso 0.590(13) 1 calc PR A 1 C49A C 0.520(5) 0.794(3) -0.082(2) 0.0342(16) Uani 0.590(13) 1 d P A 1 H49A H 0.5189 0.8452 -0.1228 0.041 Uiso 0.590(13) 1 calc PR A 1 C50A C 0.572(2) 0.6896(17) -0.0781(11) 0.0342(16) Uani 0.590(13) 1 d P A 1 H50A H 0.6123 0.6688 -0.1143 0.041 Uiso 0.590(13) 1 calc PR A 1 C51A C 0.5647(19) 0.6149(17) -0.0192(10) 0.0342(16) Uani 0.590(13) 1 d P A 1 H51A H 0.6048 0.5412 -0.0132 0.041 Uiso 0.590(13) 1 calc PR A 1 C52A C 0.499(2) 0.6468(17) 0.0311(10) 0.0342(16) Uani 0.590(13) 1 d P A 1 H52A H 0.4964 0.5943 0.0716 0.041 Uiso 0.590(13) 1 calc PR A 1 C47B C 0.4345(11) 0.7565(10) 0.0242(6) 0.0342(16) Uani 0.410(13) 1 d P A 2 C48B C 0.454(5) 0.823(5) -0.033(3) 0.0342(16) Uani 0.410(13) 1 d P A 2 H48B H 0.416 0.8969 -0.0378 0.041 Uiso 0.410(13) 1 calc PR A 2 C49B C 0.519(8) 0.807(5) -0.087(3) 0.0342(16) Uani 0.410(13) 1 d P A 2 H49B H 0.5602 0.8568 -0.1168 0.041 Uiso 0.410(13) 1 calc PR A 2 C50B C 0.513(3) 0.714(2) -0.0919(16) 0.0342(16) Uani 0.410(13) 1 d P A 2 H50B H 0.5432 0.6951 -0.1303 0.041 Uiso 0.410(13) 1 calc PR A 2 C51B C 0.466(3) 0.640(2) -0.0433(14) 0.0342(16) Uani 0.410(13) 1 d P A 2 H51B H 0.4632 0.572 -0.0493 0.041 Uiso 0.410(13) 1 calc PR A 2 C52B C 0.424(3) 0.661(2) 0.0141(15) 0.0342(16) Uani 0.410(13) 1 d P A 2 H52B H 0.3875 0.6102 0.0464 0.041 Uiso 0.410(13) 1 calc PR A 2 C53 C 0.4436(9) 0.8415(8) 0.1430(5) 0.021(2) Uani 1 1 d . A . C54 C 0.5568(10) 0.8657(9) 0.1232(5) 0.027(2) Uani 1 1 d . . . H54 H 0.5952 0.8515 0.0849 0.033 Uiso 1 1 calc R A . C55 C 0.6128(11) 0.9095(9) 0.1581(6) 0.037(3) Uani 1 1 d . A . H55 H 0.6878 0.9272 0.1427 0.044 Uiso 1 1 calc R . . C56 C 0.5617(12) 0.9283(10) 0.2154(6) 0.036(3) Uani 1 1 d . . . H56 H 0.6014 0.9585 0.239 0.044 Uiso 1 1 calc R A . C57 C 0.4529(12) 0.9026(10) 0.2376(6) 0.038(3) Uani 1 1 d . A . H57 H 0.418 0.913 0.2773 0.045 Uiso 1 1 calc R . . C58 C 0.3949(11) 0.8616(9) 0.2016(6) 0.033(3) Uani 1 1 d . . . H58 H 0.3188 0.8462 0.2169 0.039 Uiso 1 1 calc R A . C61 C 0.8236(9) 0.1005(8) 0.2505(5) 0.022(2) Uani 1 1 d . A . C62 C 0.7615(10) 0.1392(9) 0.1940(5) 0.026(2) Uani 1 1 d . . . H62 H 0.677 0.1631 0.1964 0.031 Uiso 1 1 calc R A . C63 C 0.8195(12) 0.1437(10) 0.1346(6) 0.039(3) Uani 1 1 d . A . H63 H 0.7753 0.1698 0.0969 0.047 Uiso 1 1 calc R . . C64 C 0.9440(11) 0.1095(9) 0.1307(5) 0.031(3) Uani 1 1 d . . . H64 H 0.9843 0.1137 0.0899 0.037 Uiso 1 1 calc R A . C65 C 1.0079(10) 0.0702(9) 0.1844(6) 0.032(3) Uani 1 1 d . A . H65 H 1.0922 0.0466 0.1813 0.038 Uiso 1 1 calc R . . C66 C 0.9495(10) 0.0649(9) 0.2439(5) 0.027(2) Uani 1 1 d . . . H66 H 0.9949 0.0367 0.2812 0.032 Uiso 1 1 calc R A . C67 C 0.7640(10) 0.2126(8) 0.3595(5) 0.023(2) Uani 1 1 d . A . C68 C 0.6695(11) 0.2706(9) 0.3889(5) 0.029(3) Uani 1 1 d . . . H68 H 0.5942 0.2511 0.394 0.034 Uiso 1 1 calc R A . C69 C 0.6799(14) 0.3558(10) 0.4112(6) 0.044(3) Uani 1 1 d . A . H69 H 0.6118 0.3956 0.4291 0.053 Uiso 1 1 calc R . . C70 C 0.7902(14) 0.3821(11) 0.4072(6) 0.044(3) Uani 1 1 d . . . H70 H 0.7992 0.439 0.4233 0.053 Uiso 1 1 calc R A . C71 C 0.8855(14) 0.3253(11) 0.3799(7) 0.052(4) Uani 1 1 d . A . H71 H 0.9617 0.3424 0.3772 0.062 Uiso 1 1 calc R . . C72 C 0.8724(11) 0.2422(9) 0.3560(6) 0.032(3) Uani 1 1 d . . . H72 H 0.9402 0.2046 0.3367 0.039 Uiso 1 1 calc R A . C73 C 0.8337(10) -0.0326(9) 0.3882(5) 0.025(2) Uani 1 1 d . A . C74 C 0.8655(10) -0.0377(10) 0.4486(5) 0.030(3) Uani 1 1 d . . . H74 H 0.8402 0.0249 0.4636 0.036 Uiso 1 1 calc R A . C75 C 0.9331(10) -0.1316(9) 0.4877(6) 0.030(3) Uani 1 1 d . A . H75 H 0.9565 -0.1314 0.5278 0.036 Uiso 1 1 calc R . . C76 C 0.9658(11) -0.2238(9) 0.4686(6) 0.032(3) Uani 1 1 d . . . H76 H 1.0116 -0.2883 0.4953 0.039 Uiso 1 1 calc R A . C77 C 0.9312(11) -0.2222(10) 0.4091(6) 0.038(3) Uani 1 1 d . A . H77 H 0.9517 -0.2869 0.3961 0.046 Uiso 1 1 calc R . . C78 C 0.8669(10) -0.1273(9) 0.3685(6) 0.030(3) Uani 1 1 d . . . H78 H 0.8458 -0.1269 0.3277 0.036 Uiso 1 1 calc R A . N2 N 0.3718(10) 0.4812(9) 0.3592(5) 0.044(3) Uani 1 1 d . . . Si3A Si 0.3051(7) 0.4212(6) 0.4278(3) 0.0408(15) Uani 0.621(9) 1 d P B 1 HI3A H 0.3612 0.424 0.4585 0.049 Uiso 0.621(9) 1 calc PR B 1 C3AA C 0.334(7) 0.264(3) 0.444(5) 0.100(10) Uani 0.621(9) 1 d P B 1 H3A1 H 0.4075 0.2395 0.4201 0.15 Uiso 0.621(9) 1 calc PR B 1 H3A2 H 0.2668 0.2452 0.4301 0.15 Uiso 0.621(9) 1 calc PR B 1 H3A3 H 0.3439 0.2289 0.49 0.15 Uiso 0.621(9) 1 calc PR B 1 C3BA C 0.179(3) 0.475(2) 0.4598(19) 0.100(10) Uani 0.621(9) 1 d P B 1 H3B1 H 0.1697 0.5544 0.4483 0.15 Uiso 0.621(9) 1 calc PR B 1 H3B2 H 0.1789 0.4456 0.5066 0.15 Uiso 0.621(9) 1 calc PR B 1 H3B3 H 0.1118 0.4585 0.4437 0.15 Uiso 0.621(9) 1 calc PR B 1 Si3B Si 0.2626(12) 0.3992(10) 0.4108(6) 0.0408(15) Uani 0.379(9) 1 d P B 2 HI3B H 0.2429 0.3743 0.3752 0.049 Uiso 0.379(9) 1 calc PR B 2 C3AB C 0.334(12) 0.284(6) 0.448(8) 0.100(10) Uani 0.379(9) 1 d P B 2 H3A4 H 0.4155 0.272 0.4285 0.15 Uiso 0.379(9) 1 calc PR B 2 H3A5 H 0.2943 0.2285 0.4447 0.15 Uiso 0.379(9) 1 calc PR B 2 H3A6 H 0.3377 0.2809 0.4927 0.15 Uiso 0.379(9) 1 calc PR B 2 C3BB C 0.127(5) 0.472(4) 0.418(3) 0.100(10) Uani 0.379(9) 1 d P B 2 H3B4 H 0.1224 0.547 0.3907 0.15 Uiso 0.379(9) 1 calc PR B 2 H3B5 H 0.1099 0.4732 0.4629 0.15 Uiso 0.379(9) 1 calc PR B 2 H3B6 H 0.0688 0.4406 0.4053 0.15 Uiso 0.379(9) 1 calc PR B 2 Si4 Si 0.3830(4) 0.6131(3) 0.34447(19) 0.0444(10) Uani 1 1 d . A . HI4 H 0.4208 0.6319 0.3003 0.053 Uiso 1 1 calc R . . C4A C 0.4837(17) 0.6401(13) 0.3951(9) 0.076(6) Uani 1 1 d . . . H4A1 H 0.5599 0.5871 0.3977 0.115 Uiso 1 1 calc R B . H4A2 H 0.4465 0.634 0.4382 0.115 Uiso 1 1 calc R . . H4A3 H 0.4978 0.7136 0.3761 0.115 Uiso 1 1 calc R . . C4B C 0.2399(12) 0.7137(10) 0.3396(7) 0.046(3) Uani 1 1 d . . . H4B1 H 0.186 0.6992 0.3133 0.069 Uiso 1 1 calc R B . H4B2 H 0.2543 0.787 0.3201 0.069 Uiso 1 1 calc R . . H4B3 H 0.2033 0.7083 0.3828 0.069 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 0.0150(3) 0.0145(3) 0.0166(3) -0.0032(2) -0.0018(2) -0.0034(2) O1 0.018(4) 0.024(4) 0.034(4) -0.009(3) -0.001(3) -0.007(3) O2 0.023(4) 0.021(4) 0.024(4) 0.000(3) -0.001(3) -0.003(3) N1 0.018(4) 0.016(4) 0.034(5) -0.007(4) -0.009(4) 0.001(4) C1 0.024(6) 0.011(5) 0.028(6) -0.006(4) -0.003(5) 0.001(4) C2 0.026(6) 0.016(5) 0.032(6) -0.006(4) -0.004(5) -0.005(4) C3 0.019(5) 0.021(5) 0.021(5) -0.001(4) -0.004(4) -0.002(4) Si1 0.0212(15) 0.0207(14) 0.0189(14) -0.0041(11) 0.0004(12) -0.0047(12) C4 0.029(6) 0.023(5) 0.022(6) -0.006(4) -0.006(5) 0.000(5) C5 0.027(6) 0.022(5) 0.037(7) -0.010(5) 0.000(5) -0.004(5) C6 0.014(5) 0.022(5) 0.035(6) -0.014(5) -0.003(5) 0.006(4) C7 0.036(7) 0.022(6) 0.045(8) -0.004(5) -0.004(6) -0.003(5) C8 0.026(6) 0.017(5) 0.046(7) -0.006(5) -0.004(6) 0.002(5) C9 0.021(6) 0.020(5) 0.033(6) -0.007(5) -0.002(5) -0.001(4) C10 0.031(6) 0.021(5) 0.016(5) -0.003(4) 0.000(5) -0.003(5) C11 0.011(5) 0.017(5) 0.035(6) 0.000(5) -0.006(5) 0.007(4) C12 0.029(6) 0.024(6) 0.039(7) -0.003(5) -0.011(5) -0.004(5) C13 0.032(7) 0.027(6) 0.046(8) -0.005(5) -0.021(6) -0.007(5) C14 0.019(5) 0.024(6) 0.036(6) -0.005(5) -0.001(5) -0.011(5) C15 0.012(5) 0.021(5) 0.030(6) -0.001(4) -0.002(4) -0.004(4) C21 0.016(5) 0.009(4) 0.031(6) -0.002(4) -0.004(4) 0.004(4) C22 0.020(5) 0.019(5) 0.024(6) -0.013(4) 0.003(4) 0.001(4) C23 0.017(5) 0.022(5) 0.019(5) -0.006(4) -0.003(4) -0.002(4) Si2 0.0181(15) 0.0241(15) 0.0192(15) -0.0049(12) 0.0015(12) -0.0004(12) C24 0.023(6) 0.019(5) 0.020(5) -0.003(4) 0.002(4) 0.004(4) C25 0.030(6) 0.022(5) 0.024(6) 0.002(4) 0.000(5) -0.008(5) C26 0.034(7) 0.025(6) 0.031(6) -0.002(5) 0.007(5) -0.006(5) C27 0.018(5) 0.034(6) 0.029(6) -0.012(5) 0.007(5) -0.010(5) C28 0.014(5) 0.024(6) 0.044(7) -0.014(5) -0.002(5) 0.000(4) C29 0.026(6) 0.022(5) 0.016(5) -0.009(4) 0.004(4) 0.002(4) C30 0.019(5) 0.017(5) 0.024(5) -0.006(4) 0.006(4) -0.004(4) O3 0.023(4) 0.017(4) 0.060(6) -0.006(4) 0.003(4) -0.002(3) C31 0.038(8) 0.033(7) 0.059(9) 0.009(6) -0.006(7) -0.017(6) C32 0.047(9) 0.054(9) 0.051(9) 0.005(7) 0.003(7) -0.020(7) C33 0.040(8) 0.050(8) 0.043(8) -0.011(7) -0.002(6) 0.001(7) C34 0.033(7) 0.038(7) 0.043(8) -0.001(6) 0.004(6) -0.006(6) C41 0.019(5) 0.028(6) 0.023(6) -0.008(4) 0.010(4) -0.005(5) C42 0.019(5) 0.029(6) 0.019(5) -0.001(4) 0.000(4) -0.003(5) C43 0.028(6) 0.038(7) 0.028(6) -0.001(5) -0.002(5) -0.005(5) C44 0.044(8) 0.028(6) 0.032(7) 0.000(5) -0.004(6) -0.005(6) C45 0.055(9) 0.026(6) 0.049(9) -0.014(6) 0.012(7) -0.010(6) C46 0.027(6) 0.023(6) 0.042(7) -0.005(5) 0.000(5) -0.005(5) C47A 0.040(4) 0.031(4) 0.033(4) -0.014(3) 0.008(3) -0.009(3) C48A 0.040(4) 0.031(4) 0.033(4) -0.014(3) 0.008(3) -0.009(3) C49A 0.040(4) 0.031(4) 0.033(4) -0.014(3) 0.008(3) -0.009(3) C50A 0.040(4) 0.031(4) 0.033(4) -0.014(3) 0.008(3) -0.009(3) C51A 0.040(4) 0.031(4) 0.033(4) -0.014(3) 0.008(3) -0.009(3) C52A 0.040(4) 0.031(4) 0.033(4) -0.014(3) 0.008(3) -0.009(3) C47B 0.040(4) 0.031(4) 0.033(4) -0.014(3) 0.008(3) -0.009(3) C48B 0.040(4) 0.031(4) 0.033(4) -0.014(3) 0.008(3) -0.009(3) C49B 0.040(4) 0.031(4) 0.033(4) -0.014(3) 0.008(3) -0.009(3) C50B 0.040(4) 0.031(4) 0.033(4) -0.014(3) 0.008(3) -0.009(3) C51B 0.040(4) 0.031(4) 0.033(4) -0.014(3) 0.008(3) -0.009(3) C52B 0.040(4) 0.031(4) 0.033(4) -0.014(3) 0.008(3) -0.009(3) C53 0.022(5) 0.019(5) 0.021(5) -0.003(4) 0.004(4) -0.005(4) C54 0.030(6) 0.025(6) 0.026(6) -0.008(5) -0.002(5) -0.002(5) C55 0.035(7) 0.030(6) 0.046(8) -0.003(6) -0.006(6) -0.014(6) C56 0.048(8) 0.032(7) 0.035(7) -0.012(5) -0.015(6) -0.011(6) C57 0.046(8) 0.045(8) 0.029(7) -0.023(6) -0.001(6) -0.008(6) C58 0.031(7) 0.036(7) 0.035(7) -0.013(5) 0.005(5) -0.014(5) C61 0.022(5) 0.018(5) 0.031(6) -0.014(4) 0.006(5) -0.007(4) C62 0.027(6) 0.034(6) 0.021(6) -0.016(5) 0.005(5) -0.006(5) C63 0.045(8) 0.042(7) 0.023(6) -0.005(5) -0.011(6) 0.003(6) C64 0.040(7) 0.036(7) 0.021(6) -0.014(5) 0.018(5) -0.016(6) C65 0.026(6) 0.036(7) 0.041(7) -0.022(6) 0.011(5) -0.013(5) C66 0.028(6) 0.038(7) 0.022(6) -0.014(5) 0.004(5) -0.018(5) C67 0.028(6) 0.013(5) 0.023(5) 0.003(4) -0.006(5) 0.000(4) C68 0.036(7) 0.024(6) 0.022(6) -0.004(5) 0.001(5) -0.004(5) C69 0.059(9) 0.037(7) 0.029(7) -0.012(6) -0.010(6) 0.011(7) C70 0.063(10) 0.031(7) 0.038(8) -0.003(6) -0.016(7) -0.014(7) C71 0.062(10) 0.041(8) 0.053(9) 0.002(7) -0.024(8) -0.025(8) C72 0.038(7) 0.030(6) 0.030(6) -0.009(5) -0.001(5) -0.010(5) C73 0.023(6) 0.024(5) 0.027(6) -0.005(5) -0.005(5) -0.002(5) C74 0.028(6) 0.034(6) 0.025(6) -0.012(5) -0.008(5) 0.004(5) C75 0.026(6) 0.033(6) 0.025(6) -0.002(5) 0.000(5) -0.005(5) C76 0.031(7) 0.023(6) 0.038(7) -0.004(5) 0.004(5) -0.004(5) C77 0.033(7) 0.025(6) 0.049(8) -0.013(6) 0.001(6) 0.010(5) C78 0.029(6) 0.027(6) 0.035(7) -0.014(5) 0.008(5) -0.008(5) N2 0.043(7) 0.037(6) 0.038(6) -0.006(5) 0.002(5) 0.011(5) Si3A 0.047(4) 0.042(3) 0.032(3) -0.011(2) 0.010(3) -0.013(3) C3AA 0.091(13) 0.035(10) 0.16(2) -0.029(15) 0.073(13) -0.023(12) C3BA 0.091(13) 0.035(10) 0.16(2) -0.029(15) 0.073(13) -0.023(12) Si3B 0.047(4) 0.042(3) 0.032(3) -0.011(2) 0.010(3) -0.013(3) C3AB 0.091(13) 0.035(10) 0.16(2) -0.029(15) 0.073(13) -0.023(12) C3BB 0.091(13) 0.035(10) 0.16(2) -0.029(15) 0.073(13) -0.023(12) Si4 0.047(2) 0.040(2) 0.044(2) -0.0216(18) -0.0063(18) 0.0079(18) C4A 0.100(15) 0.044(9) 0.091(14) -0.037(9) -0.046(11) 0.015(9) C4B 0.044(8) 0.038(7) 0.044(8) -0.008(6) 0.007(7) 0.003(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 2.310(7) . ? La1 O1 2.347(8) . ? La1 N2 2.374(11) . ? La1 O3 2.545(8) . ? La1 N1 2.622(9) . ? La1 C2 3.112(11) . ? La1 Si4 3.210(4) . ? O1 C2 1.343(12) . ? O2 C22 1.336(12) . ? N1 C15 1.350(13) . ? N1 C11 1.367(13) . ? C1 C2 1.388(14) . ? C1 C9 1.440(14) . ? C1 C11 1.500(14) . ? C2 C3 1.474(14) . ? C3 C4 1.373(14) . ? C3 Si1 1.882(11) . ? Si1 C53 1.859(11) . ? Si1 C41 1.892(11) . ? Si1 C47A 1.909(12) . ? C4 C10 1.412(15) . ? C4 H4 0.95 . ? C5 C6 1.361(15) . ? C5 C10 1.397(15) . ? C5 H5 0.95 . ? C6 C7 1.409(15) . ? C6 H6 0.95 . ? C7 C8 1.386(16) . ? C7 H7 0.95 . ? C8 C9 1.422(15) . ? C8 H8 0.95 . ? C9 C10 1.421(14) . ? C11 C12 1.388(15) . ? C12 C13 1.380(15) . ? C12 H12 0.95 . ? C13 C14 1.388(15) . ? C13 H13 0.95 . ? C14 C15 1.394(15) . ? C14 H14 0.95 . ? C15 C21 1.490(14) . ? C21 C22 1.399(14) . ? C21 C29 1.441(14) . ? C22 C23 1.434(14) . ? C23 C24 1.355(14) . ? C23 Si2 1.885(10) . ? Si2 C67 1.876(11) . ? Si2 C73 1.881(11) . ? Si2 C61 1.886(11) . ? C24 C30 1.419(14) . ? C24 H24 0.95 . ? C25 C26 1.366(16) . ? C25 C30 1.421(13) . ? C25 H25 0.95 . ? C26 C27 1.405(16) . ? C26 H26 0.95 . ? C27 C28 1.381(15) . ? C27 H27 0.95 . ? C28 C29 1.420(14) . ? C28 H28 0.95 . ? C29 C30 1.434(14) . ? O3 C34 1.436(14) . ? O3 C31 1.460(13) . ? C31 C32 1.525(19) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.521(19) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 C34 1.459(17) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C41 C42 1.384(15) . ? C41 C46 1.385(15) . ? C42 C43 1.395(15) . ? C42 H42 0.95 . ? C43 C44 1.390(17) . ? C43 H43 0.95 . ? C44 C45 1.383(19) . ? C44 H44 0.95 . ? C45 C46 1.414(17) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? C47A C48A 1.40(4) . ? C47A C52A 1.43(2) . ? C48A C49A 1.39(7) . ? C48A H48A 0.95 . ? C49A C50A 1.35(5) . ? C49A H49A 0.95 . ? C50A C51A 1.38(3) . ? C50A H50A 0.95 . ? C51A C52A 1.38(3) . ? C51A H51A 0.95 . ? C52A H52A 0.95 . ? C48B C49B 1.37(10) . ? C48B H48B 0.95 . ? C49B C50B 1.28(8) . ? C49B H49B 0.95 . ? C50B C51B 1.37(4) . ? C50B H50B 0.95 . ? C51B C52B 1.38(4) . ? C51B H51B 0.95 . ? C52B H52B 0.95 . ? C53 C54 1.409(15) . ? C53 C58 1.415(15) . ? C54 C55 1.377(16) . ? C54 H54 0.95 . ? C55 C56 1.390(17) . ? C55 H55 0.95 . ? C56 C57 1.376(17) . ? C56 H56 0.95 . ? C57 C58 1.384(16) . ? C57 H57 0.95 . ? C58 H58 0.95 . ? C61 C62 1.396(15) . ? C61 C66 1.421(15) . ? C62 C63 1.386(15) . ? C62 H62 0.95 . ? C63 C64 1.400(17) . ? C63 H63 0.95 . ? C64 C65 1.359(17) . ? C64 H64 0.95 . ? C65 C66 1.385(15) . ? C65 H65 0.95 . ? C66 H66 0.95 . ? C67 C72 1.385(16) . ? C67 C68 1.388(15) . ? C68 C69 1.389(17) . ? C68 H68 0.95 . ? C69 C70 1.386(19) . ? C69 H69 0.95 . ? C70 C71 1.36(2) . ? C70 H70 0.95 . ? C71 C72 1.395(17) . ? C71 H71 0.95 . ? C72 H72 0.95 . ? C73 C74 1.392(15) . ? C73 C78 1.398(15) . ? C74 C75 1.389(15) . ? C74 H74 0.95 . ? C75 C76 1.361(16) . ? C75 H75 0.95 . ? C76 C77 1.399(18) . ? C76 H76 0.95 . ? C77 C78 1.396(16) . ? C77 H77 0.95 . ? C78 H78 0.95 . ? N2 Si3A 1.670(12) . ? N2 Si4 1.709(12) . ? N2 Si3B 1.905(16) . ? Si3A C3BA 1.64(3) . ? Si3A C3AA 1.95(4) . ? Si3A HI3A 1 . ? C3AA H3A1 0.98 . ? C3AA H3A2 0.98 . ? C3AA H3A3 0.98 . ? C3BA H3B1 0.98 . ? C3BA H3B2 0.98 . ? C3BA H3B3 0.98 . ? Si3B C3AB 1.56(12) . ? Si3B C3BB 1.65(5) . ? Si3B HI3B 1 . ? C3AB H3A4 0.98 . ? C3AB H3A5 0.98 . ? C3AB H3A6 0.98 . ? C3BB H3B4 0.98 . ? C3BB H3B5 0.98 . ? C3BB H3B6 0.98 . ? Si4 C4B 1.847(13) . ? Si4 C4A 1.853(16) . ? Si4 HI4 1 . ? C4A H4A1 0.98 . ? C4A H4A2 0.98 . ? C4A H4A3 0.98 . ? C4B H4B1 0.98 . ? C4B H4B2 0.98 . ? C4B H4B3 0.98 . ? 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 112.2(3) . . ? O2 La1 N2 122.1(3) . . ? O1 La1 N2 118.5(3) . . ? O2 La1 O3 90.6(2) . . ? O1 La1 O3 86.5(3) . . ? N2 La1 O3 117.6(4) . . ? O2 La1 N1 71.7(3) . . ? O1 La1 N1 76.5(3) . . ? N2 La1 N1 94.3(4) . . ? O3 La1 N1 148.0(3) . . ? O2 La1 C2 124.7(3) . . ? O1 La1 C2 23.6(3) . . ? N2 La1 C2 96.7(3) . . ? O3 La1 C2 105.5(3) . . ? N1 La1 C2 67.2(3) . . ? O2 La1 Si4 149.5(2) . . ? O1 La1 Si4 98.06(19) . . ? N2 La1 Si4 31.3(3) . . ? O3 La1 Si4 95.0(2) . . ? N1 La1 Si4 113.9(2) . . ? C2 La1 Si4 82.6(2) . . ? C2 O1 La1 112.1(6) . . ? C22 O2 La1 125.7(6) . . ? C15 N1 C11 119.9(9) . . ? C15 N1 La1 123.4(7) . . ? C11 N1 La1 112.4(6) . . ? C2 C1 C9 121.1(9) . . ? C2 C1 C11 121.2(9) . . ? C9 C1 C11 117.2(9) . . ? O1 C2 C1 121.3(9) . . ? O1 C2 C3 119.9(9) . . ? C1 C2 C3 118.9(10) . . ? C1 C2 La1 90.7(7) . . ? C3 C2 La1 137.1(7) . . ? C4 C3 C2 117.2(9) . . ? C4 C3 Si1 118.8(8) . . ? C2 C3 Si1 124.0(8) . . ? C53 Si1 C3 111.4(5) . . ? C53 Si1 C41 103.6(5) . . ? C3 Si1 C41 107.3(5) . . ? C53 Si1 C47A 113.4(5) . . ? C3 Si1 C47A 116.5(5) . . ? C41 Si1 C47A 103.2(5) . . ? C3 C4 C10 124.8(10) . . ? C3 C4 H4 117.6 . . ? C10 C4 H4 117.6 . . ? C6 C5 C10 123.1(10) . . ? C6 C5 H5 118.5 . . ? C10 C5 H5 118.5 . . ? C5 C6 C7 118.7(10) . . ? C5 C6 H6 120.7 . . ? C7 C6 H6 120.7 . . ? C8 C7 C6 120.5(11) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 120.7(11) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 118.2(10) . . ? C10 C9 C1 119.3(10) . . ? C8 C9 C1 122.5(10) . . ? C5 C10 C4 123.6(10) . . ? C5 C10 C9 118.9(10) . . ? C4 C10 C9 117.6(10) . . ? N1 C11 C12 120.1(10) . . ? N1 C11 C1 121.7(10) . . ? C12 C11 C1 118.2(9) . . ? C13 C12 C11 121.0(11) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 117.7(11) . . ? C12 C13 H13 121.1 . . ? C14 C13 H13 121.1 . . ? C13 C14 C15 120.4(10) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? N1 C15 C14 120.5(10) . . ? N1 C15 C21 120.2(9) . . ? C14 C15 C21 119.3(9) . . ? C22 C21 C29 119.8(9) . . ? C22 C21 C15 121.4(9) . . ? C29 C21 C15 118.8(9) . . ? O2 C22 C21 120.8(9) . . ? O2 C22 C23 118.0(9) . . ? C21 C22 C23 121.2(9) . . ? C24 C23 C22 117.8(9) . . ? C24 C23 Si2 121.3(8) . . ? C22 C23 Si2 120.8(8) . . ? C67 Si2 C73 107.5(5) . . ? C67 Si2 C23 110.2(5) . . ? C73 Si2 C23 108.7(5) . . ? C67 Si2 C61 111.3(5) . . ? C73 Si2 C61 105.5(5) . . ? C23 Si2 C61 113.4(5) . . ? C23 C24 C30 124.1(10) . . ? C23 C24 H24 117.9 . . ? C30 C24 H24 117.9 . . ? C26 C25 C30 121.6(10) . . ? C26 C25 H25 119.2 . . ? C30 C25 H25 119.2 . . ? C25 C26 C27 119.2(10) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C28 C27 C26 120.8(10) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 121.8(10) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C28 C29 C30 116.8(9) . . ? C28 C29 C21 124.7(10) . . ? C30 C29 C21 118.5(9) . . ? C24 C30 C25 122.0(10) . . ? C24 C30 C29 118.2(9) . . ? C25 C30 C29 119.7(9) . . ? C34 O3 C31 109.2(9) . . ? C34 O3 La1 122.3(7) . . ? C31 O3 La1 118.7(7) . . ? O3 C31 C32 103.9(10) . . ? O3 C31 H31A 111 . . ? C32 C31 H31A 111 . . ? O3 C31 H31B 111 . . ? C32 C31 H31B 111 . . ? H31A C31 H31B 109 . . ? C33 C32 C31 104.7(11) . . ? C33 C32 H32A 110.8 . . ? C31 C32 H32A 110.8 . . ? C33 C32 H32B 110.8 . . ? C31 C32 H32B 110.8 . . ? H32A C32 H32B 108.9 . . ? C34 C33 C32 101.3(11) . . ? C34 C33 H33A 111.5 . . ? C32 C33 H33A 111.5 . . ? C34 C33 H33B 111.5 . . ? C32 C33 H33B 111.5 . . ? H33A C33 H33B 109.3 . . ? O3 C34 C33 105.7(10) . . ? O3 C34 H34A 110.6 . . ? C33 C34 H34A 110.6 . . ? O3 C34 H34B 110.6 . . ? C33 C34 H34B 110.6 . . ? H34A C34 H34B 108.7 . . ? C42 C41 C46 117.5(10) . . ? C42 C41 Si1 120.6(8) . . ? C46 C41 Si1 121.2(9) . . ? C41 C42 C43 122.1(11) . . ? C41 C42 H42 118.9 . . ? C43 C42 H42 118.9 . . ? C44 C43 C42 119.8(12) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C45 C44 C43 119.4(11) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C44 C45 C46 119.6(12) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C41 C46 C45 121.5(12) . . ? C41 C46 H46 119.2 . . ? C45 C46 H46 119.2 . . ? C48A C47A C52A 115(2) . . ? C48A C47A Si1 118.0(17) . . ? C52A C47A Si1 124.3(11) . . ? C49A C48A C47A 116(3) . . ? C49A C48A H48A 122 . . ? C47A C48A H48A 122 . . ? C50A C49A C48A 126(4) . . ? C50A C49A H49A 116.9 . . ? C48A C49A H49A 116.9 . . ? C49A C50A C51A 116(3) . . ? C49A C50A H50A 121.9 . . ? C51A C50A H50A 121.9 . . ? C50A C51A C52A 120.3(19) . . ? C50A C51A H51A 119.8 . . ? C52A C51A H51A 119.8 . . ? C51A C52A C47A 122.1(18) . . ? C51A C52A H52A 118.9 . . ? C47A C52A H52A 118.9 . . ? C49B C48B H48B 113.4 . . ? C50B C49B C48B 109(5) . . ? C50B C49B H49B 125.7 . . ? C48B C49B H49B 125.7 . . ? C49B C50B C51B 122(4) . . ? C49B C50B H50B 118.8 . . ? C51B C50B H50B 118.7 . . ? C50B C51B C52B 122(3) . . ? C50B C51B H51B 119.2 . . ? C52B C51B H51B 119.2 . . ? C51B C52B H52B 120.4 . . ? C54 C53 C58 115.6(10) . . ? C54 C53 Si1 124.7(8) . . ? C58 C53 Si1 119.0(8) . . ? C55 C54 C53 121.3(11) . . ? C55 C54 H54 119.4 . . ? C53 C54 H54 119.4 . . ? C54 C55 C56 121.3(11) . . ? C54 C55 H55 119.3 . . ? C56 C55 H55 119.3 . . ? C57 C56 C55 119.3(11) . . ? C57 C56 H56 120.3 . . ? C55 C56 H56 120.3 . . ? C56 C57 C58 119.4(11) . . ? C56 C57 H57 120.3 . . ? C58 C57 H57 120.3 . . ? C57 C58 C53 123.1(11) . . ? C57 C58 H58 118.5 . . ? C53 C58 H58 118.5 . . ? C62 C61 C66 116.5(10) . . ? C62 C61 Si2 123.3(8) . . ? C66 C61 Si2 120.2(8) . . ? C63 C62 C61 121.8(11) . . ? C63 C62 H62 119.1 . . ? C61 C62 H62 119.1 . . ? C62 C63 C64 119.4(11) . . ? C62 C63 H63 120.3 . . ? C64 C63 H63 120.3 . . ? C65 C64 C63 120.7(10) . . ? C65 C64 H64 119.6 . . ? C63 C64 H64 119.6 . . ? C64 C65 C66 119.8(11) . . ? C64 C65 H65 120.1 . . ? C66 C65 H65 120.1 . . ? C65 C66 C61 121.8(11) . . ? C65 C66 H66 119.1 . . ? C61 C66 H66 119.1 . . ? C72 C67 C68 115.5(10) . . ? C72 C67 Si2 122.1(9) . . ? C68 C67 Si2 122.2(9) . . ? C67 C68 C69 123.1(12) . . ? C67 C68 H68 118.4 . . ? C69 C68 H68 118.4 . . ? C70 C69 C68 119.5(13) . . ? C70 C69 H69 120.3 . . ? C68 C69 H69 120.3 . . ? C71 C70 C69 118.9(13) . . ? C71 C70 H70 120.5 . . ? C69 C70 H70 120.5 . . ? C70 C71 C72 120.7(14) . . ? C70 C71 H71 119.7 . . ? C72 C71 H71 119.7 . . ? C67 C72 C71 122.2(13) . . ? C67 C72 H72 118.9 . . ? C71 C72 H72 118.9 . . ? C74 C73 C78 118.0(10) . . ? C74 C73 Si2 123.2(9) . . ? C78 C73 Si2 118.8(9) . . ? C75 C74 C73 121.9(11) . . ? C75 C74 H74 119.1 . . ? C73 C74 H74 119.1 . . ? C76 C75 C74 120.2(12) . . ? C76 C75 H75 119.9 . . ? C74 C75 H75 119.9 . . ? C75 C76 C77 119.1(11) . . ? C75 C76 H76 120.5 . . ? C77 C76 H76 120.5 . . ? C78 C77 C76 121.2(11) . . ? C78 C77 H77 119.4 . . ? C76 C77 H77 119.4 . . ? C77 C78 C73 119.5(12) . . ? C77 C78 H78 120.2 . . ? C73 C78 H78 120.2 . . ? Si3A N2 Si4 119.3(7) . . ? Si4 N2 Si3B 132.9(7) . . ? Si3A N2 La1 138.2(7) . . ? Si4 N2 La1 102.4(5) . . ? Si3B N2 La1 119.2(7) . . ? C3BA Si3A N2 125.6(13) . . ? C3BA Si3A C3AA 115(2) . . ? N2 Si3A C3AA 112(2) . . ? C3BA Si3A HI3A 98.9 . . ? N2 Si3A HI3A 98.9 . . ? C3AA Si3A HI3A 98.9 . . ? Si3A C3AA H3A1 109.5 . . ? Si3A C3AA H3A2 109.5 . . ? H3A1 C3AA H3A2 109.5 . . ? Si3A C3AA H3A3 109.5 . . ? H3A1 C3AA H3A3 109.5 . . ? H3A2 C3AA H3A3 109.5 . . ? Si3A C3BA H3B1 109.5 . . ? Si3A C3BA H3B2 109.5 . . ? H3B1 C3BA H3B2 109.5 . . ? Si3A C3BA H3B3 109.5 . . ? H3B1 C3BA H3B3 109.5 . . ? H3B2 C3BA H3B3 109.5 . . ? C3AB Si3B C3BB 135(4) . . ? C3AB Si3B N2 109(4) . . ? C3BB Si3B N2 113.8(19) . . ? C3AB Si3B HI3B 94.4 . . ? C3BB Si3B HI3B 94.4 . . ? N2 Si3B HI3B 94.4 . . ? Si3B C3AB H3A4 109.5 . . ? Si3B C3AB H3A5 109.5 . . ? H3A4 C3AB H3A5 109.5 . . ? Si3B C3AB H3A6 109.5 . . ? H3A4 C3AB H3A6 109.5 . . ? H3A5 C3AB H3A6 109.5 . . ? Si3B C3BB H3B4 109.5 . . ? Si3B C3BB H3B5 109.5 . . ? H3B4 C3BB H3B5 109.5 . . ? Si3B C3BB H3B6 109.5 . . ? H3B4 C3BB H3B6 109.5 . . ? H3B5 C3BB H3B6 109.5 . . ? N2 Si4 C4B 115.6(6) . . ? N2 Si4 C4A 116.9(7) . . ? C4B Si4 C4A 109.2(7) . . ? N2 Si4 La1 46.2(4) . . ? C4B Si4 La1 125.8(5) . . ? C4A Si4 La1 124.5(5) . . ? N2 Si4 HI4 104.6 . . ? C4B Si4 HI4 104.6 . . ? C4A Si4 HI4 104.6 . . ? La1 Si4 HI4 58.4 . . ? Si4 C4A H4A1 109.5 . . ? Si4 C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? Si4 C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? Si4 C4B H4B1 109.5 . . ? Si4 C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? Si4 C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 La1 O1 C2 126.9(6) . . . . ? N2 La1 O1 C2 -24.2(8) . . . . ? O3 La1 O1 C2 -143.9(6) . . . . ? N1 La1 O1 C2 63.4(6) . . . . ? Si4 La1 O1 C2 -49.4(6) . . . . ? O1 La1 O2 C22 -120.8(8) . . . . ? N2 La1 O2 C22 29.0(9) . . . . ? O3 La1 O2 C22 152.7(8) . . . . ? N1 La1 O2 C22 -54.5(8) . . . . ? C2 La1 O2 C22 -97.9(8) . . . . ? Si4 La1 O2 C22 51.9(10) . . . . ? O2 La1 N1 C15 10.7(8) . . . . ? O1 La1 N1 C15 130.0(9) . . . . ? N2 La1 N1 C15 -111.7(9) . . . . ? O3 La1 N1 C15 70.2(10) . . . . ? C2 La1 N1 C15 152.8(9) . . . . ? Si4 La1 N1 C15 -137.1(8) . . . . ? O2 La1 N1 C11 -146.1(8) . . . . ? O1 La1 N1 C11 -26.8(7) . . . . ? N2 La1 N1 C11 91.5(8) . . . . ? O3 La1 N1 C11 -86.6(8) . . . . ? C2 La1 N1 C11 -3.9(7) . . . . ? Si4 La1 N1 C11 66.1(8) . . . . ? La1 O1 C2 C1 -53.0(12) . . . . ? La1 O1 C2 C3 128.4(9) . . . . ? C9 C1 C2 O1 168.2(10) . . . . ? C11 C1 C2 O1 -20.0(17) . . . . ? C9 C1 C2 C3 -13.2(16) . . . . ? C11 C1 C2 C3 158.6(10) . . . . ? C9 C1 C2 La1 134.3(10) . . . . ? C11 C1 C2 La1 -53.9(10) . . . . ? O2 La1 C2 O1 -64.2(7) . . . . ? N2 La1 C2 O1 158.8(7) . . . . ? O3 La1 C2 O1 37.6(7) . . . . ? N1 La1 C2 O1 -109.4(7) . . . . ? Si4 La1 C2 O1 130.7(6) . . . . ? O2 La1 C2 C1 72.7(7) . . . . ? O1 La1 C2 C1 136.9(10) . . . . ? N2 La1 C2 C1 -64.3(7) . . . . ? O3 La1 C2 C1 174.5(6) . . . . ? N1 La1 C2 C1 27.6(6) . . . . ? Si4 La1 C2 C1 -92.3(6) . . . . ? O2 La1 C2 C3 -151.0(10) . . . . ? O1 La1 C2 C3 -86.8(12) . . . . ? N2 La1 C2 C3 71.9(11) . . . . ? O3 La1 C2 C3 -49.2(11) . . . . ? N1 La1 C2 C3 163.8(12) . . . . ? Si4 La1 C2 C3 43.9(11) . . . . ? O1 C2 C3 C4 -171.8(10) . . . . ? C1 C2 C3 C4 9.6(16) . . . . ? La1 C2 C3 C4 -118.2(11) . . . . ? O1 C2 C3 Si1 5.9(15) . . . . ? C1 C2 C3 Si1 -172.8(8) . . . . ? La1 C2 C3 Si1 59.4(14) . . . . ? C4 C3 Si1 C53 94.0(9) . . . . ? C2 C3 Si1 C53 -83.6(10) . . . . ? C4 C3 Si1 C41 -18.7(10) . . . . ? C2 C3 Si1 C41 163.7(9) . . . . ? C4 C3 Si1 C47A -133.7(9) . . . . ? C2 C3 Si1 C47A 48.7(11) . . . . ? C2 C3 C4 C10 -0.4(17) . . . . ? Si1 C3 C4 C10 -178.2(9) . . . . ? C10 C5 C6 C7 1.1(18) . . . . ? C5 C6 C7 C8 -1.1(18) . . . . ? C6 C7 C8 C9 0.7(19) . . . . ? C7 C8 C9 C10 -0.2(18) . . . . ? C7 C8 C9 C1 177.6(11) . . . . ? C2 C1 C9 C10 7.5(17) . . . . ? C11 C1 C9 C10 -164.6(10) . . . . ? C2 C1 C9 C8 -170.2(11) . . . . ? C11 C1 C9 C8 17.7(16) . . . . ? C6 C5 C10 C4 179.9(11) . . . . ? C6 C5 C10 C9 -0.6(18) . . . . ? C3 C4 C10 C5 174.2(11) . . . . ? C3 C4 C10 C9 -5.2(17) . . . . ? C8 C9 C10 C5 0.1(16) . . . . ? C1 C9 C10 C5 -177.7(10) . . . . ? C8 C9 C10 C4 179.6(10) . . . . ? C1 C9 C10 C4 1.8(16) . . . . ? C15 N1 C11 C12 -0.5(16) . . . . ? La1 N1 C11 C12 157.1(9) . . . . ? C15 N1 C11 C1 -179.5(10) . . . . ? La1 N1 C11 C1 -21.9(13) . . . . ? C2 C1 C11 N1 65.0(15) . . . . ? C9 C1 C11 N1 -122.9(11) . . . . ? C2 C1 C11 C12 -114.0(13) . . . . ? C9 C1 C11 C12 58.1(14) . . . . ? N1 C11 C12 C13 -3.6(18) . . . . ? C1 C11 C12 C13 175.4(11) . . . . ? C11 C12 C13 C14 2.9(19) . . . . ? C12 C13 C14 C15 1.7(18) . . . . ? C11 N1 C15 C14 5.2(16) . . . . ? La1 N1 C15 C14 -149.9(8) . . . . ? C11 N1 C15 C21 -175.0(9) . . . . ? La1 N1 C15 C21 29.9(13) . . . . ? C13 C14 C15 N1 -5.9(16) . . . . ? C13 C14 C15 C21 174.3(10) . . . . ? N1 C15 C21 C22 -49.8(15) . . . . ? C14 C15 C21 C22 130.0(11) . . . . ? N1 C15 C21 C29 130.1(11) . . . . ? C14 C15 C21 C29 -50.0(14) . . . . ? La1 O2 C22 C21 57.7(13) . . . . ? La1 O2 C22 C23 -123.9(8) . . . . ? C29 C21 C22 O2 -174.0(9) . . . . ? C15 C21 C22 O2 6.0(16) . . . . ? C29 C21 C22 C23 7.7(15) . . . . ? C15 C21 C22 C23 -172.4(10) . . . . ? O2 C22 C23 C24 175.1(9) . . . . ? C21 C22 C23 C24 -6.5(15) . . . . ? O2 C22 C23 Si2 -2.2(13) . . . . ? C21 C22 C23 Si2 176.2(8) . . . . ? C24 C23 Si2 C67 -114.5(9) . . . . ? C22 C23 Si2 C67 62.7(9) . . . . ? C24 C23 Si2 C73 3.0(10) . . . . ? C22 C23 Si2 C73 -179.8(8) . . . . ? C24 C23 Si2 C61 120.0(9) . . . . ? C22 C23 Si2 C61 -62.8(9) . . . . ? C22 C23 C24 C30 1.5(16) . . . . ? Si2 C23 C24 C30 178.7(8) . . . . ? C30 C25 C26 C27 -3.5(18) . . . . ? C25 C26 C27 C28 1.8(18) . . . . ? C26 C27 C28 C29 1.9(17) . . . . ? C27 C28 C29 C30 -3.7(16) . . . . ? C27 C28 C29 C21 178.6(10) . . . . ? C22 C21 C29 C28 173.9(10) . . . . ? C15 C21 C29 C28 -6.0(16) . . . . ? C22 C21 C29 C30 -3.8(15) . . . . ? C15 C21 C29 C30 176.3(9) . . . . ? C23 C24 C30 C25 -178.7(10) . . . . ? C23 C24 C30 C29 2.2(16) . . . . ? C26 C25 C30 C24 -177.5(11) . . . . ? C26 C25 C30 C29 1.6(17) . . . . ? C28 C29 C30 C24 -178.9(9) . . . . ? C21 C29 C30 C24 -1.1(15) . . . . ? C28 C29 C30 C25 2.0(15) . . . . ? C21 C29 C30 C25 179.8(10) . . . . ? O2 La1 O3 C34 5.5(9) . . . . ? O1 La1 O3 C34 -106.8(9) . . . . ? N2 La1 O3 C34 132.7(9) . . . . ? N1 La1 O3 C34 -49.5(11) . . . . ? C2 La1 O3 C34 -121.0(9) . . . . ? Si4 La1 O3 C34 155.4(8) . . . . ? O2 La1 O3 C31 147.5(9) . . . . ? O1 La1 O3 C31 35.2(9) . . . . ? N2 La1 O3 C31 -85.3(9) . . . . ? N1 La1 O3 C31 92.6(10) . . . . ? C2 La1 O3 C31 21.1(9) . . . . ? Si4 La1 O3 C31 -62.6(9) . . . . ? C34 O3 C31 C32 5.9(14) . . . . ? La1 O3 C31 C32 -140.7(9) . . . . ? O3 C31 C32 C33 18.1(15) . . . . ? C31 C32 C33 C34 -34.7(15) . . . . ? C31 O3 C34 C33 -28.9(14) . . . . ? La1 O3 C34 C33 116.2(10) . . . . ? C32 C33 C34 O3 38.8(14) . . . . ? C53 Si1 C41 C42 176.9(8) . . . . ? C3 Si1 C41 C42 -65.2(9) . . . . ? C47A Si1 C41 C42 58.4(9) . . . . ? C53 Si1 C41 C46 7.0(10) . . . . ? C3 Si1 C41 C46 124.9(9) . . . . ? C47A Si1 C41 C46 -111.5(10) . . . . ? C46 C41 C42 C43 1.0(16) . . . . ? Si1 C41 C42 C43 -169.3(8) . . . . ? C41 C42 C43 C44 0.3(17) . . . . ? C42 C43 C44 C45 -1.0(18) . . . . ? C43 C44 C45 C46 0.5(19) . . . . ? C42 C41 C46 C45 -1.6(17) . . . . ? Si1 C41 C46 C45 168.6(9) . . . . ? C44 C45 C46 C41 0.9(19) . . . . ? C53 Si1 C47A C48A -78.8(19) . . . . ? C3 Si1 C47A C48A 149.9(19) . . . . ? C41 Si1 C47A C48A 32.6(19) . . . . ? C53 Si1 C47A C52A 82.0(15) . . . . ? C3 Si1 C47A C52A -49.3(16) . . . . ? C41 Si1 C47A C52A -166.6(14) . . . . ? C52A C47A C48A C49A 23(4) . . . . ? Si1 C47A C48A C49A -174(3) . . . . ? C47A C48A C49A C50A -20(7) . . . . ? C48A C49A C50A C51A 5(7) . . . . ? C49A C50A C51A C52A 4(4) . . . . ? C50A C51A C52A C47A 1(3) . . . . ? C48A C47A C52A C51A -16(3) . . . . ? Si1 C47A C52A C51A -177.1(16) . . . . ? C48B C49B C50B C51B -10(9) . . . . ? C49B C50B C51B C52B -1(7) . . . . ? C3 Si1 C53 C54 155.3(9) . . . . ? C41 Si1 C53 C54 -89.6(9) . . . . ? C47A Si1 C53 C54 21.5(11) . . . . ? C3 Si1 C53 C58 -35.1(10) . . . . ? C41 Si1 C53 C58 80.0(9) . . . . ? C47A Si1 C53 C58 -168.9(9) . . . . ? C58 C53 C54 C55 -2.1(16) . . . . ? Si1 C53 C54 C55 167.8(9) . . . . ? C53 C54 C55 C56 2.1(18) . . . . ? C54 C55 C56 C57 -0.1(19) . . . . ? C55 C56 C57 C58 -1.8(19) . . . . ? C56 C57 C58 C53 1.8(19) . . . . ? C54 C53 C58 C57 0.2(17) . . . . ? Si1 C53 C58 C57 -170.3(10) . . . . ? C67 Si2 C61 C62 -100.0(9) . . . . ? C73 Si2 C61 C62 143.8(9) . . . . ? C23 Si2 C61 C62 24.9(10) . . . . ? C67 Si2 C61 C66 79.6(9) . . . . ? C73 Si2 C61 C66 -36.7(9) . . . . ? C23 Si2 C61 C66 -155.5(8) . . . . ? C66 C61 C62 C63 -0.6(16) . . . . ? Si2 C61 C62 C63 178.9(9) . . . . ? C61 C62 C63 C64 -0.5(18) . . . . ? C62 C63 C64 C65 1.1(18) . . . . ? C63 C64 C65 C66 -0.6(18) . . . . ? C64 C65 C66 C61 -0.6(17) . . . . ? C62 C61 C66 C65 1.2(15) . . . . ? Si2 C61 C66 C65 -178.4(8) . . . . ? C73 Si2 C67 C72 67.0(10) . . . . ? C23 Si2 C67 C72 -174.8(9) . . . . ? C61 Si2 C67 C72 -48.1(10) . . . . ? C73 Si2 C67 C68 -108.2(9) . . . . ? C23 Si2 C67 C68 10.1(10) . . . . ? C61 Si2 C67 C68 136.8(9) . . . . ? C72 C67 C68 C69 2.6(16) . . . . ? Si2 C67 C68 C69 178.0(9) . . . . ? C67 C68 C69 C70 -3.2(18) . . . . ? C68 C69 C70 C71 1.6(19) . . . . ? C69 C70 C71 C72 0(2) . . . . ? C68 C67 C72 C71 -0.5(17) . . . . ? Si2 C67 C72 C71 -175.9(10) . . . . ? C70 C71 C72 C67 -1(2) . . . . ? C67 Si2 C73 C74 18.7(11) . . . . ? C23 Si2 C73 C74 -100.5(10) . . . . ? C61 Si2 C73 C74 137.6(10) . . . . ? C67 Si2 C73 C78 -161.2(9) . . . . ? C23 Si2 C73 C78 79.5(9) . . . . ? C61 Si2 C73 C78 -42.4(10) . . . . ? C78 C73 C74 C75 3.1(17) . . . . ? Si2 C73 C74 C75 -176.9(9) . . . . ? C73 C74 C75 C76 -3.0(18) . . . . ? C74 C75 C76 C77 0.4(17) . . . . ? C75 C76 C77 C78 1.9(18) . . . . ? C76 C77 C78 C73 -1.7(18) . . . . ? C74 C73 C78 C77 -0.8(16) . . . . ? Si2 C73 C78 C77 179.2(9) . . . . ? O2 La1 N2 Si3A -24.5(12) . . . . ? O1 La1 N2 Si3A 123.6(9) . . . . ? O3 La1 N2 Si3A -134.5(9) . . . . ? N1 La1 N2 Si3A 46.7(10) . . . . ? C2 La1 N2 Si3A 114.1(10) . . . . ? Si4 La1 N2 Si3A 177.8(14) . . . . ? O2 La1 N2 Si4 157.7(4) . . . . ? O1 La1 N2 Si4 -54.2(6) . . . . ? O3 La1 N2 Si4 47.7(6) . . . . ? N1 La1 N2 Si4 -131.1(5) . . . . ? C2 La1 N2 Si4 -63.7(5) . . . . ? O2 La1 N2 Si3B -45.0(8) . . . . ? O1 La1 N2 Si3B 103.1(7) . . . . ? O3 La1 N2 Si3B -155.0(6) . . . . ? N1 La1 N2 Si3B 26.1(7) . . . . ? C2 La1 N2 Si3B 93.6(7) . . . . ? Si4 La1 N2 Si3B 157.2(11) . . . . ? Si4 N2 Si3A C3BA 45(2) . . . . ? Si3B N2 Si3A C3BA -85(2) . . . . ? La1 N2 Si3A C3BA -132.6(19) . . . . ? Si4 N2 Si3A C3AA -166(4) . . . . ? Si3B N2 Si3A C3AA 63(4) . . . . ? La1 N2 Si3A C3AA 16(4) . . . . ? Si3A N2 Si3B C3AB -72(7) . . . . ? Si4 N2 Si3B C3AB -137(7) . . . . ? La1 N2 Si3B C3AB 74(7) . . . . ? Si3A N2 Si3B C3BB 95(3) . . . . ? Si4 N2 Si3B C3BB 30(3) . . . . ? La1 N2 Si3B C3BB -119(3) . . . . ? Si3A N2 Si4 C4B -62.2(10) . . . . ? Si3B N2 Si4 C4B -36.4(13) . . . . ? La1 N2 Si4 C4B 116.2(6) . . . . ? Si3A N2 Si4 C4A 68.4(11) . . . . ? Si3B N2 Si4 C4A 94.2(13) . . . . ? La1 N2 Si4 C4A -113.2(8) . . . . ? Si3A N2 Si4 La1 -178.3(11) . . . . ? Si3B N2 Si4 La1 -152.5(13) . . . . ? O2 La1 Si4 N2 -39.2(7) . . . . ? O1 La1 Si4 N2 134.0(6) . . . . ? O3 La1 Si4 N2 -138.9(6) . . . . ? N1 La1 Si4 N2 55.2(6) . . . . ? C2 La1 Si4 N2 116.1(6) . . . . ? O2 La1 Si4 C4B -131.8(6) . . . . ? O1 La1 Si4 C4B 41.4(6) . . . . ? N2 La1 Si4 C4B -92.6(8) . . . . ? O3 La1 Si4 C4B 128.6(6) . . . . ? N1 La1 Si4 C4B -37.3(6) . . . . ? C2 La1 Si4 C4B 23.6(6) . . . . ? O2 La1 Si4 C4A 56.6(9) . . . . ? O1 La1 Si4 C4A -130.2(8) . . . . ? N2 La1 Si4 C4A 95.8(10) . . . . ? O3 La1 Si4 C4A -43.0(8) . . . . ? N1 La1 Si4 C4A 151.1(8) . . . . ? C2 La1 Si4 C4A -148.0(8) . . . . ? #===END data_complex4 _database_code_depnum_ccdc_archive 'CCDC 752788' #TrackingRef 'Cif_files_B920283H.cif' _audit_creation_date 2009-02-04T16:56:05-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety "C45 H65 N2 O3 Sc Si4, 2.5(C6 H6)'" _chemical_formula_sum 'C60 H80 N2 O3 Sc Si4' _chemical_formula_weight 1034.58 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2092(6) _cell_length_b 23.4248(12) _cell_length_c 22.6197(11) _cell_angle_alpha 90 _cell_angle_beta 94.018(3) _cell_angle_gamma 90 _cell_volume 5924.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7551 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.34 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.16 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2220 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 0.940 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_unetI/netI 0.0491 _diffrn_reflns_number 63479 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 13476 _reflns_number_gt 11736 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART, 2006' _computing_cell_refinement 'Bruker SMART, 2006' _computing_data_reduction 'Bruker SAINT, 2006' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0167P)^2^+8.1396P] 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_number_reflns 13476 _refine_ls_number_parameters 565 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.528 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.06 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Sc1 Sc 0.53122(4) 0.173728(17) 0.805469(17) 0.01343(9) Uani 1 1 d . . . O3 O 0.68370(14) 0.22816(7) 0.78899(6) 0.0174(3) Uani 1 1 d . B . C31 C 0.7866(2) 0.22768(11) 0.83273(10) 0.0222(5) Uani 1 1 d . . . H31A H 0.8286 0.1905 0.8322 0.027 Uiso 1 1 calc R B . H31B H 0.7605 0.2344 0.8731 0.027 Uiso 1 1 calc R . . C32 C 0.8657(3) 0.27446(17) 0.81510(18) 0.0664(12) Uani 1 1 d . B . H32A H 0.8571 0.3081 0.841 0.08 Uiso 1 1 calc R . . H32B H 0.9502 0.2619 0.8189 0.08 Uiso 1 1 calc R . . C33 C 0.8316(3) 0.28916(16) 0.75448(14) 0.0529(10) Uani 1 1 d . . . H33A H 0.8867 0.2711 0.7277 0.064 Uiso 1 1 calc R B . H33B H 0.8348 0.3311 0.7491 0.064 Uiso 1 1 calc R . . C34 C 0.7060(2) 0.26779(10) 0.74062(10) 0.0216(5) Uani 1 1 d . B . H34A H 0.6482 0.2998 0.7394 0.026 Uiso 1 1 calc R . . H34B H 0.6992 0.2479 0.7019 0.026 Uiso 1 1 calc R . . N1 N 0.42116(16) 0.10958(8) 0.85687(8) 0.0153(4) Uani 1 1 d . B . O1 O 0.64586(13) 0.10728(6) 0.80289(6) 0.0161(3) Uani 1 1 d . B . C2 C 0.60881(19) 0.05655(9) 0.78059(9) 0.0154(4) Uani 1 1 d . . . C3 C 0.6764(2) 0.02862(10) 0.73659(10) 0.0183(5) Uani 1 1 d . A . C4 C 0.6300(2) -0.02080(10) 0.71163(10) 0.0206(5) Uani 1 1 d . . . H4 H 0.6746 -0.0399 0.6834 0.025 Uiso 1 1 calc R B . C10 C 0.5191(2) -0.04498(10) 0.72568(10) 0.0189(5) Uani 1 1 d . B . C5 C 0.4697(2) -0.09331(10) 0.69518(11) 0.0246(5) Uani 1 1 d . . . H5 H 0.5131 -0.1109 0.6655 0.03 Uiso 1 1 calc R B . C6 C 0.3611(2) -0.11521(11) 0.70755(11) 0.0272(6) Uani 1 1 d . B . H6 H 0.3294 -0.1477 0.6868 0.033 Uiso 1 1 calc R . . C7 C 0.2970(2) -0.08890(10) 0.75164(12) 0.0265(5) Uani 1 1 d . . . H7 H 0.2209 -0.1035 0.7599 0.032 Uiso 1 1 calc R B . C8 C 0.3428(2) -0.04255(10) 0.78281(11) 0.0222(5) Uani 1 1 d . B . H8 H 0.2982 -0.0259 0.8126 0.027 Uiso 1 1 calc R . . C9 C 0.4558(2) -0.01912(9) 0.77116(10) 0.0168(4) Uani 1 1 d . . . C1 C 0.50591(19) 0.03094(9) 0.80042(9) 0.0155(4) Uani 1 1 d . B . C11 C 0.45196(19) 0.05327(9) 0.85404(10) 0.0163(4) Uani 1 1 d . . . C12 C 0.4362(2) 0.01619(10) 0.90098(10) 0.0199(5) Uani 1 1 d . B . H12 H 0.4579 -0.0229 0.8981 0.024 Uiso 1 1 calc R . . C13 C 0.3890(2) 0.03643(10) 0.95182(10) 0.0228(5) Uani 1 1 d . . . H13 H 0.3825 0.0121 0.985 0.027 Uiso 1 1 calc R B . Si1 Si 0.82419(6) 0.05567(3) 0.71197(3) 0.02123(14) Uani 1 1 d . . . C42 C 0.8237(2) 0.13406(10) 0.69710(12) 0.0295(6) Uani 1 1 d . A . H42A H 0.9015 0.1455 0.6837 0.044 Uiso 1 1 calc R . . H42B H 0.8088 0.1547 0.7335 0.044 Uiso 1 1 calc R . . H42C H 0.7607 0.1431 0.6663 0.044 Uiso 1 1 calc R . . C41 C 0.8522(3) 0.02064(12) 0.63955(11) 0.0322(6) Uani 1 1 d . A . H41A H 0.7861 0.0294 0.6103 0.048 Uiso 1 1 calc R . . H41B H 0.8579 -0.0208 0.6451 0.048 Uiso 1 1 calc R . . H41C H 0.9272 0.035 0.6254 0.048 Uiso 1 1 calc R . . C43A C 0.9491(2) 0.03483(11) 0.76918(12) 0.0287(6) Uani 0.533(6) 1 d P A 1 C44A C 0.9300(5) -0.0266(3) 0.7867(3) 0.0362(10) Uani 0.533(6) 1 d P A 1 H44A H 0.998 -0.0395 0.813 0.054 Uiso 0.533(6) 1 calc PR A 1 H44B H 0.9234 -0.0505 0.7511 0.054 Uiso 0.533(6) 1 calc PR A 1 H44C H 0.8563 -0.0296 0.8074 0.054 Uiso 0.533(6) 1 calc PR A 1 C45A C 1.0659(5) 0.0402(3) 0.7356(3) 0.0362(10) Uani 0.533(6) 1 d P A 1 H45A H 1.0733 0.0792 0.7208 0.054 Uiso 0.533(6) 1 calc PR A 1 H45B H 1.0623 0.0134 0.7022 0.054 Uiso 0.533(6) 1 calc PR A 1 H45C H 1.1353 0.0311 0.7627 0.054 Uiso 0.533(6) 1 calc PR A 1 C46A C 0.9501(5) 0.0758(3) 0.8183(2) 0.0362(10) Uani 0.533(6) 1 d P A 1 H46A H 0.8708 0.0769 0.834 0.054 Uiso 0.533(6) 1 calc PR A 1 H46B H 0.9705 0.1138 0.804 0.054 Uiso 0.533(6) 1 calc PR A 1 H46C H 1.0096 0.064 0.8497 0.054 Uiso 0.533(6) 1 calc PR A 1 C43B C 0.9491(2) 0.03483(11) 0.76918(12) 0.0287(6) Uani 0.467(6) 1 d P A 2 C44B C 0.9797(6) -0.0297(3) 0.7692(3) 0.0329(11) Uani 0.467(6) 1 d P A 2 H44D H 1.0181 -0.0393 0.7329 0.049 Uiso 0.467(6) 1 calc PR A 2 H44E H 0.9061 -0.052 0.771 0.049 Uiso 0.467(6) 1 calc PR A 2 H44F H 1.0343 -0.0386 0.8037 0.049 Uiso 0.467(6) 1 calc PR A 2 C45B C 1.0694(5) 0.0677(3) 0.7659(3) 0.0329(11) Uani 0.467(6) 1 d P A 2 H45D H 1.13 0.051 0.794 0.049 Uiso 0.467(6) 1 calc PR A 2 H45E H 1.0576 0.1079 0.776 0.049 Uiso 0.467(6) 1 calc PR A 2 H45F H 1.0961 0.065 0.7257 0.049 Uiso 0.467(6) 1 calc PR A 2 C46B C 0.9136(5) 0.0461(3) 0.8366(3) 0.0329(11) Uani 0.467(6) 1 d P A 2 H46D H 0.9823 0.0374 0.8644 0.049 Uiso 0.467(6) 1 calc PR A 2 H46E H 0.8462 0.0214 0.8452 0.049 Uiso 0.467(6) 1 calc PR A 2 H46F H 0.8907 0.0861 0.841 0.049 Uiso 0.467(6) 1 calc PR A 2 O2 O 0.50810(13) 0.22266(6) 0.87658(6) 0.0162(3) Uani 1 1 d . B . C22 C 0.40193(19) 0.23336(9) 0.89866(9) 0.0153(4) Uani 1 1 d . . . C23 C 0.3713(2) 0.29130(9) 0.91399(9) 0.0164(4) Uani 1 1 d . B . C24 C 0.2586(2) 0.30085(10) 0.93285(9) 0.0181(5) Uani 1 1 d . . . H24 H 0.2376 0.3387 0.9429 0.022 Uiso 1 1 calc R B . C30 C 0.1720(2) 0.25704(10) 0.93802(9) 0.0172(4) Uani 1 1 d . B . C25 C 0.0563(2) 0.26933(11) 0.95651(10) 0.0216(5) Uani 1 1 d . . . H25 H 0.0355 0.3076 0.9652 0.026 Uiso 1 1 calc R B . C26 C -0.0258(2) 0.22651(11) 0.96192(10) 0.0241(5) Uani 1 1 d . B . H26 H -0.1021 0.235 0.9755 0.029 Uiso 1 1 calc R . . C27 C 0.0035(2) 0.16998(11) 0.94737(10) 0.0239(5) Uani 1 1 d . . . H27 H -0.0544 0.1406 0.9498 0.029 Uiso 1 1 calc R B . C28 C 0.1152(2) 0.15694(11) 0.92966(11) 0.0229(5) Uani 1 1 d . B . H28 H 0.1331 0.1186 0.9199 0.027 Uiso 1 1 calc R . . C29 C 0.2043(2) 0.19965(10) 0.92567(10) 0.0184(5) Uani 1 1 d . . . C21 C 0.3234(2) 0.18836(10) 0.90825(10) 0.0174(5) Uani 1 1 d . B . C15 C 0.36589(19) 0.12844(10) 0.90535(10) 0.0172(5) Uani 1 1 d . . . C14 C 0.3515(2) 0.09240(10) 0.95372(10) 0.0209(5) Uani 1 1 d . B . H14 H 0.3159 0.1065 0.9877 0.025 Uiso 1 1 calc R . . Si2 Si 0.47986(6) 0.35294(3) 0.91484(3) 0.01831(14) Uani 1 1 d . . . C51 C 0.3926(2) 0.42155(10) 0.91574(12) 0.0286(6) Uani 1 1 d . B . H51A H 0.4479 0.454 0.916 0.043 Uiso 1 1 calc R . . H51B H 0.3476 0.4228 0.9513 0.043 Uiso 1 1 calc R . . H51C H 0.337 0.4235 0.8804 0.043 Uiso 1 1 calc R . . C52 C 0.5667(2) 0.35249(10) 0.84716(11) 0.0256(5) Uani 1 1 d . B . H52A H 0.5115 0.3561 0.8118 0.038 Uiso 1 1 calc R . . H52B H 0.611 0.3166 0.8454 0.038 Uiso 1 1 calc R . . H52C H 0.6229 0.3846 0.8489 0.038 Uiso 1 1 calc R . . C53 C 0.5837(2) 0.34874(12) 0.98510(11) 0.0272(6) Uani 1 1 d . B . C56 C 0.6420(3) 0.28953(15) 0.99125(14) 0.0517(9) Uani 1 1 d . . . H56A H 0.6941 0.2881 1.0278 0.078 Uiso 1 1 calc R B . H56B H 0.6893 0.2824 0.9572 0.078 Uiso 1 1 calc R . . H56C H 0.5796 0.2603 0.9926 0.078 Uiso 1 1 calc R . . C55 C 0.6818(3) 0.39452(18) 0.98384(16) 0.0698(13) Uani 1 1 d . . . H55A H 0.6448 0.4324 0.981 0.105 Uiso 1 1 calc R B . H55B H 0.7288 0.3882 0.9495 0.105 Uiso 1 1 calc R . . H55C H 0.7343 0.3922 1.0203 0.105 Uiso 1 1 calc R . . C54 C 0.5120(3) 0.35789(15) 1.03943(12) 0.0468(8) Uani 1 1 d . . . H54A H 0.4473 0.3297 1.0393 0.07 Uiso 1 1 calc R B . H54B H 0.478 0.3964 1.0383 0.07 Uiso 1 1 calc R . . H54C H 0.5648 0.3533 1.0755 0.07 Uiso 1 1 calc R . . N61 N 0.42342(18) 0.19171(9) 0.73072(9) 0.0235(4) Uani 1 1 d . B . Si4A Si 0.31715(10) 0.24413(4) 0.73243(4) 0.0567(3) Uani 0.652(5) 1 d P B 1 H4SA H 0.351(3) 0.2802(13) 0.7773(13) 0.05 Uiso 0.65 1 d P B 1 C4A1 C 0.1647(4) 0.2099(3) 0.7603(3) 0.066 Uani 0.65 1 d P B 1 H4A1 H 0.1302 0.1834 0.7302 0.099 Uiso 0.652(5) 1 calc PR B 1 H4A2 H 0.1073 0.2404 0.7668 0.099 Uiso 0.652(5) 1 calc PR B 1 H4A3 H 0.183 0.1892 0.7975 0.099 Uiso 0.652(5) 1 calc PR B 1 C4B1 C 0.2711(6) 0.2795(2) 0.6652(2) 0.0642(17) Uani 0.652(5) 1 d P B 1 H4B1 H 0.3403 0.2979 0.6491 0.096 Uiso 0.652(5) 1 calc PR B 1 H4B2 H 0.2108 0.3083 0.6728 0.096 Uiso 0.652(5) 1 calc PR B 1 H4B3 H 0.2368 0.2516 0.6365 0.096 Uiso 0.652(5) 1 calc PR B 1 Si4B Si 0.31715(10) 0.24413(4) 0.73243(4) 0.0567(3) Uani 0.348(5) 1 d P B 2 H4SB H 0.351(3) 0.2802(13) 0.7773(13) 0.05 Uiso 0.35 1 d P B 2 C4A2 C 0.1766(8) 0.2332(5) 0.7063(5) 0.066 Uani 0.35 1 d P B 2 H4A4 H 0.1751 0.2229 0.6642 0.099 Uiso 0.348(5) 1 calc PR B 2 H4A5 H 0.1299 0.2681 0.7108 0.099 Uiso 0.348(5) 1 calc PR B 2 H4A6 H 0.1419 0.202 0.7284 0.099 Uiso 0.348(5) 1 calc PR B 2 C4B2 C 0.3812(12) 0.3052(4) 0.6691(4) 0.0642(17) Uani 0.348(5) 1 d P B 2 H4B4 H 0.3918 0.2859 0.6314 0.096 Uiso 0.348(5) 1 calc PR B 2 H4B5 H 0.4579 0.3211 0.6847 0.096 Uiso 0.348(5) 1 calc PR B 2 H4B6 H 0.3227 0.3361 0.6627 0.096 Uiso 0.348(5) 1 calc PR B 2 Si3 Si 0.43854(6) 0.14789(3) 0.67049(3) 0.02360(15) Uani 1 1 d . B . H3S H 0.547(3) 0.1151(13) 0.6835(13) 0.05 Uiso 1 1 d . . . C3A C 0.3121(2) 0.09668(13) 0.65784(12) 0.034 Uani 1 1 d . . . H3A1 H 0.3062 0.073 0.6932 0.051 Uiso 1 1 calc R B . H3A2 H 0.3263 0.0722 0.6239 0.051 Uiso 1 1 calc R . . H3A3 H 0.2374 0.1179 0.6497 0.051 Uiso 1 1 calc R . . C3B C 0.4655(3) 0.18556(15) 0.59991(13) 0.0453(8) Uani 1 1 d . . . H3B1 H 0.3939 0.2072 0.5864 0.068 Uiso 1 1 calc R B . H3B2 H 0.4836 0.1575 0.5697 0.068 Uiso 1 1 calc R . . H3B3 H 0.5332 0.2118 0.6066 0.068 Uiso 1 1 calc R . . C101 C 0.7097(3) 0.32244(13) 0.58342(12) 0.039 Uani 1 1 d . . . H101 H 0.6342 0.3079 0.5689 0.047 Uiso 1 1 calc R . . C102 C 0.8115(3) 0.29054(12) 0.57812(12) 0.041 Uani 1 1 d . . . H102 H 0.8061 0.2541 0.5597 0.05 Uiso 1 1 calc R . . C103 C 0.9212(3) 0.31125(12) 0.59949(12) 0.037 Uani 1 1 d . . . H103 H 0.9912 0.289 0.596 0.044 Uiso 1 1 calc R . . C104 C 0.9297(3) 0.36448(12) 0.62604(11) 0.032 Uani 1 1 d . . . H104 H 1.0056 0.3788 0.6405 0.038 Uiso 1 1 calc R . . C105 C 0.8280(3) 0.39691(12) 0.63162(11) 0.032 Uani 1 1 d . . . H105 H 0.8337 0.4333 0.6501 0.038 Uiso 1 1 calc R . . C106 C 0.7176(3) 0.37591(13) 0.61007(11) 0.034 Uani 1 1 d . . . H106 H 0.6474 0.3981 0.6135 0.041 Uiso 1 1 calc R . . C111 C 0.7359(2) 0.06967(14) 0.94652(13) 0.04 Uani 1 1 d . . . H111 H 0.7071 0.0639 0.9065 0.049 Uiso 1 1 calc R . . C112 C 0.8219(3) 0.03312(14) 0.97268(15) 0.045 Uani 1 1 d . . . H112 H 0.8515 0.0023 0.9507 0.054 Uiso 1 1 calc R . . C113 C 0.8639(3) 0.04181(15) 1.03070(15) 0.05 Uani 1 1 d . . . H113 H 0.9226 0.0169 1.0488 0.06 Uiso 1 1 calc R . . C114 C 0.8211(3) 0.08644(17) 1.06241(14) 0.053 Uani 1 1 d . . . H114 H 0.8506 0.0924 1.1023 0.064 Uiso 1 1 calc R . . C115 C 0.7348(3) 0.12290(16) 1.03648(15) 0.049 Uani 1 1 d . . . H115 H 0.7053 0.1537 1.0586 0.059 Uiso 1 1 calc R . . C116 C 0.6920(2) 0.11431(15) 0.97856(14) 0.042 Uani 1 1 d . . . H116 H 0.6327 0.139 0.9607 0.051 Uiso 1 1 calc R . . C122 C 0.5253(3) 0.01948(15) 0.55729(13) 0.046 Uani 1 1 d . . . H122 H 0.5428 0.0329 0.5966 0.055 Uiso 1 1 calc R . . C123 C 0.4393(3) -0.02204(15) 0.54597(13) 0.046 Uani 1 1 d . . . H123 H 0.3975 -0.0372 0.5775 0.055 Uiso 1 1 calc R . . C121 C 0.5861(3) 0.04160(15) 0.51105(14) 0.047 Uani 1 1 d . . . H121 H 0.6452 0.0702 0.5187 0.056 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 Sc1 0.0120(2) 0.0139(2) 0.01453(18) 0.00140(16) 0.00197(15) 0.00024(16) O3 0.0175(8) 0.0185(8) 0.0163(7) 0.0039(6) 0.0015(6) -0.0024(6) C31 0.0183(12) 0.0271(13) 0.0207(11) 0.0017(10) -0.0017(9) -0.0020(10) C32 0.041(2) 0.071(3) 0.082(3) 0.047(2) -0.0266(19) -0.0361(18) C33 0.048(2) 0.072(2) 0.0377(16) 0.0220(16) -0.0045(15) -0.0390(18) C34 0.0253(13) 0.0211(12) 0.0192(11) 0.0072(9) 0.0066(10) -0.0021(10) N1 0.0128(9) 0.0155(9) 0.0179(9) 0.0009(7) 0.0033(7) -0.0010(7) O1 0.0142(8) 0.0154(8) 0.0189(7) -0.0002(6) 0.0031(6) 0.0002(6) C2 0.0159(11) 0.0149(11) 0.0150(10) 0.0018(8) -0.0011(8) 0.0006(8) C3 0.0187(12) 0.0172(11) 0.0195(11) 0.0027(9) 0.0043(9) 0.0025(9) C4 0.0248(13) 0.0185(11) 0.0191(11) 0.0015(9) 0.0044(10) 0.0050(10) C10 0.0209(12) 0.0159(11) 0.0195(11) 0.0015(9) -0.0015(9) 0.0030(9) C5 0.0296(14) 0.0190(12) 0.0244(12) -0.0029(10) -0.0032(10) 0.0035(10) C6 0.0274(14) 0.0197(12) 0.0330(13) -0.0019(11) -0.0082(11) -0.0010(10) C7 0.0195(12) 0.0207(12) 0.0388(14) 0.0027(11) -0.0031(11) -0.0031(10) C8 0.0202(12) 0.0181(12) 0.0285(12) 0.0019(10) 0.0019(10) 0.0031(9) C9 0.0167(11) 0.0137(11) 0.0196(10) 0.0034(9) -0.0006(9) 0.0045(8) C1 0.0161(11) 0.0136(10) 0.0168(10) 0.0024(8) 0.0010(9) 0.0013(8) C11 0.0118(10) 0.0161(11) 0.0213(11) 0.0003(9) 0.0037(9) -0.0017(8) C12 0.0192(12) 0.0161(11) 0.0249(11) 0.0037(9) 0.0038(10) -0.0005(9) C13 0.0235(13) 0.0220(12) 0.0238(12) 0.0066(10) 0.0083(10) -0.0025(10) Si1 0.0219(3) 0.0174(3) 0.0258(3) 0.0012(3) 0.0122(3) 0.0025(3) C42 0.0285(14) 0.0217(13) 0.0404(15) 0.0012(11) 0.0166(12) 0.0013(10) C41 0.0413(16) 0.0282(14) 0.0295(13) 0.0026(11) 0.0193(12) 0.0054(12) C43A 0.0209(13) 0.0279(14) 0.0383(14) 0.0023(11) 0.0099(11) 0.0020(10) C44A 0.0239(17) 0.047(2) 0.0369(19) 0.0048(15) -0.0025(14) 0.0047(14) C45A 0.0239(17) 0.047(2) 0.0369(19) 0.0048(15) -0.0025(14) 0.0047(14) C46A 0.0239(17) 0.047(2) 0.0369(19) 0.0048(15) -0.0025(14) 0.0047(14) C43B 0.0209(13) 0.0279(14) 0.0383(14) 0.0023(11) 0.0099(11) 0.0020(10) C44B 0.0226(19) 0.038(2) 0.038(2) 0.0040(16) 0.0008(15) 0.0039(15) C45B 0.0226(19) 0.038(2) 0.038(2) 0.0040(16) 0.0008(15) 0.0039(15) C46B 0.0226(19) 0.038(2) 0.038(2) 0.0040(16) 0.0008(15) 0.0039(15) O2 0.0130(8) 0.0181(8) 0.0180(7) -0.0003(6) 0.0043(6) -0.0003(6) C22 0.0139(11) 0.0195(11) 0.0127(9) -0.0003(8) 0.0010(8) 0.0019(9) C23 0.0166(11) 0.0174(11) 0.0150(10) -0.0001(9) 0.0004(9) 0.0007(9) C24 0.0199(12) 0.0178(11) 0.0163(10) -0.0027(9) -0.0008(9) 0.0019(9) C30 0.0147(11) 0.0213(12) 0.0153(10) -0.0013(9) -0.0004(9) 0.0016(9) C25 0.0191(12) 0.0276(13) 0.0183(11) -0.0043(10) 0.0026(9) 0.0048(10) C26 0.0148(12) 0.0364(14) 0.0214(11) -0.0032(10) 0.0040(9) 0.0026(10) C27 0.0167(12) 0.0322(14) 0.0233(11) -0.0042(10) 0.0042(10) -0.0053(10) C28 0.0178(12) 0.0234(12) 0.0281(12) -0.0057(10) 0.0062(10) -0.0034(10) C29 0.0145(11) 0.0228(12) 0.0181(10) -0.0019(9) 0.0034(9) 0.0000(9) C21 0.0175(11) 0.0173(11) 0.0179(10) -0.0011(9) 0.0040(9) 0.0003(9) C15 0.0125(11) 0.0176(11) 0.0221(11) -0.0009(9) 0.0051(9) -0.0024(8) C14 0.0206(12) 0.0213(12) 0.0221(11) 0.0015(9) 0.0102(10) -0.0011(9) Si2 0.0188(3) 0.0167(3) 0.0196(3) -0.0018(2) 0.0027(3) -0.0012(2) C51 0.0287(14) 0.0193(12) 0.0387(14) -0.0015(11) 0.0084(12) -0.0008(10) C52 0.0330(14) 0.0180(12) 0.0269(12) -0.0013(10) 0.0101(11) -0.0040(10) C53 0.0252(13) 0.0333(14) 0.0222(12) -0.0030(11) -0.0031(10) -0.0059(11) C56 0.050(2) 0.066(2) 0.0357(16) -0.0105(16) -0.0210(15) 0.0258(17) C55 0.063(2) 0.091(3) 0.051(2) 0.012(2) -0.0240(19) -0.053(2) C54 0.053(2) 0.064(2) 0.0229(13) -0.0074(14) -0.0008(14) 0.0050(17) N61 0.0222(11) 0.0224(11) 0.0251(10) 0.0041(8) -0.0050(9) -0.0002(8) Si4A 0.0649(7) 0.0438(5) 0.0546(6) -0.0253(5) -0.0435(5) 0.0333(5) C4A1 0.018 0.1 0.08 -0.046 -0.007 0.014 C4B1 0.099(4) 0.041(3) 0.047(3) -0.008(2) -0.032(3) 0.040(3) Si4B 0.0649(7) 0.0438(5) 0.0546(6) -0.0253(5) -0.0435(5) 0.0333(5) C4A2 0.018 0.1 0.08 -0.046 -0.007 0.014 C4B2 0.099(4) 0.041(3) 0.047(3) -0.008(2) -0.032(3) 0.040(3) Si3 0.0215(3) 0.0308(4) 0.0185(3) 0.0062(3) 0.0016(3) -0.0001(3) C3A 0.032 0.043 0.026 -0.007 0.001 -0.006 C3B 0.0504(19) 0.055(2) 0.0316(15) 0.0189(14) 0.0128(14) 0.0051(16) C101 0.048 0.043 0.025 0.007 -0.007 -0.022 C102 0.069 0.027 0.027 -0.003 -0.004 -0.009 C103 0.048 0.032 0.03 -0.001 0.005 0.002 C104 0.037 0.029 0.028 0.002 0.002 -0.008 C105 0.04 0.026 0.028 -0.003 0.001 -0.008 C106 0.037 0.039 0.027 0.003 0.002 -0.006 C111 0.024 0.062 0.034 0.019 -0.004 -0.018 C112 0.031 0.044 0.06 0.015 0.003 -0.013 C113 0.03 0.058 0.06 0.029 -0.009 -0.004 C114 0.038 0.082 0.037 0.019 -0.012 -0.015 C115 0.035 0.068 0.045 0.007 0.003 -0.005 C116 0.021 0.061 0.045 0.02 -0.001 -0.006 C122 0.044 0.067 0.026 0 0.001 0.008 C123 0.042 0.066 0.03 0.013 0.007 0.01 C121 0.043 0.056 0.041 0.006 0.001 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sc1 O2 2.0067(15) . ? Sc1 O1 2.0218(15) . ? Sc1 N61 2.052(2) . ? Sc1 O3 2.1852(16) . ? Sc1 N1 2.3094(18) . ? Sc1 Si3 3.2130(8) . ? Sc1 Si4A 3.2637(9) . ? O3 C31 1.466(3) . ? O3 C34 1.470(3) . ? C31 C32 1.482(4) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.439(4) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 C34 1.506(4) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? N1 C11 1.366(3) . ? N1 C15 1.370(3) . ? O1 C2 1.345(3) . ? C2 C1 1.401(3) . ? C2 C3 1.449(3) . ? C3 C4 1.374(3) . ? C3 Si1 1.893(2) . ? C4 C10 1.423(3) . ? C4 H4 0.95 . ? C10 C5 1.418(3) . ? C10 C9 1.425(3) . ? C5 C6 1.368(4) . ? C5 H5 0.95 . ? C6 C7 1.411(4) . ? C6 H6 0.95 . ? C7 C8 1.374(3) . ? C7 H7 0.95 . ? C8 C9 1.422(3) . ? C8 H8 0.95 . ? C9 C1 1.441(3) . ? C1 C11 1.488(3) . ? C11 C12 1.392(3) . ? C12 C13 1.383(3) . ? C12 H12 0.95 . ? C13 C14 1.379(3) . ? C13 H13 0.95 . ? Si1 C42 1.867(3) . ? Si1 C41 1.878(3) . ? Si1 C43A 1.903(3) . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C43A C46A 1.467(6) . ? C43A C44A 1.512(6) . ? C43A C45A 1.564(6) . ? C44A H44A 0.98 . ? C44A H44B 0.98 . ? C44A H44C 0.98 . ? C45A H45A 0.98 . ? C45A H45B 0.98 . ? C45A H45C 0.98 . ? C46A H46A 0.98 . ? C46A H46B 0.98 . ? C46A H46C 0.98 . ? C44B H44D 0.98 . ? C44B H44E 0.98 . ? C44B H44F 0.98 . ? C45B H45D 0.98 . ? C45B H45E 0.98 . ? C45B H45F 0.98 . ? C46B H46D 0.98 . ? C46B H46E 0.98 . ? C46B H46F 0.98 . ? O2 C22 1.346(2) . ? C22 C21 1.400(3) . ? C22 C23 1.448(3) . ? C23 C24 1.380(3) . ? C23 Si2 1.888(2) . ? C24 C30 1.422(3) . ? C24 H24 0.95 . ? C30 C25 1.420(3) . ? C30 C29 1.425(3) . ? C25 C26 1.372(3) . ? C25 H25 0.95 . ? C26 C27 1.409(3) . ? C26 H26 0.95 . ? C27 C28 1.375(3) . ? C27 H27 0.95 . ? C28 C29 1.421(3) . ? C28 H28 0.95 . ? C29 C21 1.443(3) . ? C21 C15 1.485(3) . ? C15 C14 1.400(3) . ? C14 H14 0.95 . ? Si2 C52 1.870(2) . ? Si2 C51 1.882(3) . ? Si2 C53 1.906(3) . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? C53 C54 1.530(4) . ? C53 C56 1.535(4) . ? C53 C55 1.537(4) . ? C56 H56A 0.98 . ? C56 H56B 0.98 . ? C56 H56C 0.98 . ? C55 H55A 0.98 . ? C55 H55B 0.98 . ? C55 H55C 0.98 . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? N61 Si4A 1.713(2) . ? N61 Si3 1.724(2) . ? Si4A C4B1 1.777(5) . ? Si4A C4A1 2.028(6) . ? Si4A H4SA 1.36(3) . ? Si4A H4SB 1.36(3) . ? C4A1 H4A1 0.98 . ? C4A1 H4A2 0.98 . ? C4A1 H4A3 0.98 . ? C4B1 H4B1 0.98 . ? C4B1 H4B2 0.98 . ? C4B1 H4B3 0.98 . ? C4A2 H4A4 0.98 . ? C4A2 H4A5 0.98 . ? C4A2 H4A6 0.98 . ? C4B2 H4B4 0.98 . ? C4B2 H4B5 0.98 . ? C4B2 H4B6 0.98 . ? Si3 C3A 1.863(3) . ? Si3 C3B 1.867(3) . ? Si3 H3S 1.45(3) . ? C3A H3A1 0.98 . ? C3A H3A2 0.98 . ? C3A H3A3 0.98 . ? C3B H3B1 0.98 . ? C3B H3B2 0.98 . ? C3B H3B3 0.98 . ? C101 C102 1.376(4) . ? C101 C106 1.390(4) . ? C101 H101 0.95 . ? C102 C103 1.377(4) . ? C102 H102 0.95 . ? C103 C104 1.384(4) . ? C103 H103 0.95 . ? C104 C105 1.383(4) . ? C104 H104 0.95 . ? C105 C106 1.388(4) . ? C105 H105 0.95 . ? C106 H106 0.95 . ? C111 C116 1.382(5) . ? C111 C112 1.390(4) . ? C111 H111 0.95 . ? C112 C113 1.378(5) . ? C112 H112 0.95 . ? C113 C114 1.373(5) . ? C113 H113 0.95 . ? C114 C115 1.389(5) . ? C114 H114 0.95 . ? C115 C116 1.378(4) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C122 C123 1.381(5) . ? C122 C121 1.388(4) . ? C122 H122 0.95 . ? C123 C121 1.380(4) 3_656 ? C123 H123 0.95 . ? C121 C123 1.380(4) 3_656 ? C121 H121 0.95 . ? 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 Sc1 O1 125.51(6) . . ? O2 Sc1 N61 116.21(7) . . ? O1 Sc1 N61 118.23(7) . . ? O2 Sc1 O3 87.13(6) . . ? O1 Sc1 O3 86.44(6) . . ? N61 Sc1 O3 99.33(7) . . ? O2 Sc1 N1 82.22(6) . . ? O1 Sc1 N1 82.91(6) . . ? N61 Sc1 N1 104.12(7) . . ? O3 Sc1 N1 156.54(6) . . ? O2 Sc1 Si3 144.88(5) . . ? O1 Sc1 Si3 89.51(5) . . ? N61 Sc1 Si3 28.72(6) . . ? O3 Sc1 Si3 98.77(4) . . ? N1 Sc1 Si3 101.97(5) . . ? O2 Sc1 Si4A 89.17(5) . . ? O1 Sc1 Si4A 145.15(5) . . ? N61 Sc1 Si4A 27.06(6) . . ? O3 Sc1 Si4A 100.07(5) . . ? N1 Sc1 Si4A 100.60(5) . . ? Si3 Sc1 Si4A 55.72(2) . . ? C31 O3 C34 109.90(16) . . ? C31 O3 Sc1 117.91(12) . . ? C34 O3 Sc1 132.19(13) . . ? O3 C31 C32 105.7(2) . . ? O3 C31 H31A 110.6 . . ? C32 C31 H31A 110.6 . . ? O3 C31 H31B 110.6 . . ? C32 C31 H31B 110.6 . . ? H31A C31 H31B 108.7 . . ? C33 C32 C31 108.0(3) . . ? C33 C32 H32A 110.1 . . ? C31 C32 H32A 110.1 . . ? C33 C32 H32B 110.1 . . ? C31 C32 H32B 110.1 . . ? H32A C32 H32B 108.4 . . ? C32 C33 C34 107.5(2) . . ? C32 C33 H33A 110.2 . . ? C34 C33 H33A 110.2 . . ? C32 C33 H33B 110.2 . . ? C34 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? O3 C34 C33 105.10(19) . . ? O3 C34 H34A 110.7 . . ? C33 C34 H34A 110.7 . . ? O3 C34 H34B 110.7 . . ? C33 C34 H34B 110.7 . . ? H34A C34 H34B 108.8 . . ? C11 N1 C15 118.62(18) . . ? C11 N1 Sc1 117.33(13) . . ? C15 N1 Sc1 118.72(14) . . ? C2 O1 Sc1 120.71(13) . . ? O1 C2 C1 119.85(19) . . ? O1 C2 C3 119.59(19) . . ? C1 C2 C3 120.6(2) . . ? C4 C3 C2 117.5(2) . . ? C4 C3 Si1 118.35(17) . . ? C2 C3 Si1 124.16(17) . . ? C3 C4 C10 123.7(2) . . ? C3 C4 H4 118.1 . . ? C10 C4 H4 118.1 . . ? C5 C10 C4 121.8(2) . . ? C5 C10 C9 119.6(2) . . ? C4 C10 C9 118.6(2) . . ? C6 C5 C10 121.5(2) . . ? C6 C5 H5 119.3 . . ? C10 C5 H5 119.3 . . ? C5 C6 C7 119.0(2) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C8 C7 C6 121.1(2) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 121.0(2) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C8 C9 C10 117.7(2) . . ? C8 C9 C1 123.5(2) . . ? C10 C9 C1 118.7(2) . . ? C2 C1 C9 120.3(2) . . ? C2 C1 C11 120.1(2) . . ? C9 C1 C11 119.55(19) . . ? N1 C11 C12 121.4(2) . . ? N1 C11 C1 119.75(19) . . ? C12 C11 C1 118.8(2) . . ? C13 C12 C11 119.8(2) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C14 C13 C12 119.2(2) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C42 Si1 C41 105.74(12) . . ? C42 Si1 C3 113.01(11) . . ? C41 Si1 C3 108.27(12) . . ? C42 Si1 C43A 111.56(13) . . ? C41 Si1 C43A 108.72(12) . . ? C3 Si1 C43A 109.35(11) . . ? Si1 C42 H42A 109.5 . . ? Si1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 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 . . ? C46A C43A C44A 114.7(4) . . ? C46A C43A C45A 110.7(4) . . ? C44A C43A C45A 110.0(4) . . ? C46A C43A Si1 108.3(3) . . ? C44A C43A Si1 108.2(3) . . ? C45A C43A Si1 104.5(2) . . ? H44D C44B H44E 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? H45D C45B H45E 109.5 . . ? H45D C45B H45F 109.5 . . ? H45E C45B H45F 109.5 . . ? H46D C46B H46E 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? C22 O2 Sc1 124.81(13) . . ? O2 C22 C21 119.94(19) . . ? O2 C22 C23 119.62(19) . . ? C21 C22 C23 120.41(19) . . ? C24 C23 C22 117.6(2) . . ? C24 C23 Si2 118.47(17) . . ? C22 C23 Si2 123.75(16) . . ? C23 C24 C30 123.6(2) . . ? C23 C24 H24 118.2 . . ? C30 C24 H24 118.2 . . ? C25 C30 C24 121.3(2) . . ? C25 C30 C29 119.9(2) . . ? C24 C30 C29 118.7(2) . . ? C26 C25 C30 120.7(2) . . ? C26 C25 H25 119.7 . . ? C30 C25 H25 119.7 . . ? C25 C26 C27 119.9(2) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 120.5(2) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 121.4(2) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C28 C29 C30 117.5(2) . . ? C28 C29 C21 123.8(2) . . ? C30 C29 C21 118.6(2) . . ? C22 C21 C29 120.5(2) . . ? C22 C21 C15 119.86(19) . . ? C29 C21 C15 119.4(2) . . ? N1 C15 C14 121.0(2) . . ? N1 C15 C21 120.31(19) . . ? C14 C15 C21 118.71(19) . . ? C13 C14 C15 119.8(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C52 Si2 C51 108.31(12) . . ? C52 Si2 C23 111.06(10) . . ? C51 Si2 C23 108.55(11) . . ? C52 Si2 C53 111.10(12) . . ? C51 Si2 C53 108.81(12) . . ? C23 Si2 C53 108.95(11) . . ? Si2 C51 H51A 109.5 . . ? Si2 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si2 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si2 C52 H52A 109.5 . . ? Si2 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si2 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C56 107.3(2) . . ? C54 C53 C55 109.5(3) . . ? C56 C53 C55 109.4(3) . . ? C54 C53 Si2 109.77(19) . . ? C56 C53 Si2 110.69(18) . . ? C55 C53 Si2 110.1(2) . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Si4A N61 Si3 123.48(12) . . ? Si4A N61 Sc1 119.92(11) . . ? Si3 N61 Sc1 116.38(11) . . ? N61 Si4A C4B1 118.4(2) . . ? N61 Si4A C4A1 109.0(2) . . ? C4B1 Si4A C4A1 104.5(3) . . ? C4B1 Si4A Sc1 145.9(2) . . ? C4A1 Si4A Sc1 104.36(19) . . ? N61 Si4A H4SA 107.6(13) . . ? C4B1 Si4A H4SA 113.6(13) . . ? C4A1 Si4A H4SA 102.4(13) . . ? Sc1 Si4A H4SA 77.1(13) . . ? N61 Si4A H4SB 107.6(13) . . ? C4B1 Si4A H4SB 113.6(13) . . ? C4A1 Si4A H4SB 102.4(13) . . ? Sc1 Si4A H4SB 77.1(13) . . ? H4A4 C4A2 H4A5 109.5 . . ? H4A4 C4A2 H4A6 109.5 . . ? H4A5 C4A2 H4A6 109.5 . . ? H4B4 C4B2 H4B5 109.5 . . ? H4B4 C4B2 H4B6 109.5 . . ? H4B5 C4B2 H4B6 109.5 . . ? N61 Si3 C3A 112.88(11) . . ? N61 Si3 C3B 115.17(13) . . ? C3A Si3 C3B 109.87(14) . . ? C3A Si3 Sc1 117.32(9) . . ? C3B Si3 Sc1 131.50(12) . . ? N61 Si3 H3S 106.4(12) . . ? C3A Si3 H3S 108.0(12) . . ? C3B Si3 H3S 103.9(12) . . ? Sc1 Si3 H3S 72.3(12) . . ? Si3 C3A H3A1 109.5 . . ? Si3 C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? Si3 C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? Si3 C3B H3B1 109.5 . . ? Si3 C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? Si3 C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C102 C101 C106 120.0(3) . . ? C102 C101 H101 120 . . ? C106 C101 H101 120 . . ? C101 C102 C103 120.2(3) . . ? C101 C102 H102 119.9 . . ? C103 C102 H102 119.9 . . ? C102 C103 C104 120.2(3) . . ? C102 C103 H103 119.9 . . ? C104 C103 H103 119.9 . . ? C105 C104 C103 120.1(3) . . ? C105 C104 H104 119.9 . . ? C103 C104 H104 119.9 . . ? C104 C105 C106 119.6(3) . . ? C104 C105 H105 120.2 . . ? C106 C105 H105 120.2 . . ? C105 C106 C101 120.0(3) . . ? C105 C106 H106 120 . . ? C101 C106 H106 120 . . ? C116 C111 C112 120.3(3) . . ? C116 C111 H111 119.9 . . ? C112 C111 H111 119.9 . . ? C113 C112 C111 119.7(3) . . ? C113 C112 H112 120.2 . . ? C111 C112 H112 120.2 . . ? C114 C113 C112 120.1(3) . . ? C114 C113 H113 120 . . ? C112 C113 H113 120 . . ? C113 C114 C115 120.4(3) . . ? C113 C114 H114 119.8 . . ? C115 C114 H114 119.8 . . ? C116 C115 C114 119.8(3) . . ? C116 C115 H115 120.1 . . ? C114 C115 H115 120.1 . . ? C115 C116 C111 119.8(3) . . ? C115 C116 H116 120.1 . . ? C111 C116 H116 120.1 . . ? C123 C122 C121 119.8(3) . . ? C123 C122 H122 120.1 . . ? C121 C122 H122 120.1 . . ? C121 C123 C122 120.2(3) 3_656 . ? C121 C123 H123 119.9 3_656 . ? C122 C123 H123 119.9 . . ? C123 C121 C122 120.0(3) 3_656 . ? C123 C121 H121 120 3_656 . ? C122 C121 H121 120 . . ? 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 Sc1 O3 C31 64.95(15) . . . . ? O1 Sc1 O3 C31 -60.91(15) . . . . ? N61 Sc1 O3 C31 -178.95(15) . . . . ? N1 Sc1 O3 C31 2.1(2) . . . . ? Si3 Sc1 O3 C31 -149.87(14) . . . . ? Si4A Sc1 O3 C31 153.59(14) . . . . ? O2 Sc1 O3 C34 -114.58(18) . . . . ? O1 Sc1 O3 C34 119.56(18) . . . . ? N61 Sc1 O3 C34 1.51(19) . . . . ? N1 Sc1 O3 C34 -177.44(18) . . . . ? Si3 Sc1 O3 C34 30.60(18) . . . . ? Si4A Sc1 O3 C34 -25.94(18) . . . . ? C34 O3 C31 C32 8.4(3) . . . . ? Sc1 O3 C31 C32 -171.3(2) . . . . ? O3 C31 C32 C33 -17.7(4) . . . . ? C31 C32 C33 C34 20.2(4) . . . . ? C31 O3 C34 C33 3.6(3) . . . . ? Sc1 O3 C34 C33 -176.87(19) . . . . ? C32 C33 C34 O3 -14.6(4) . . . . ? O2 Sc1 N1 C11 -142.52(16) . . . . ? O1 Sc1 N1 C11 -15.09(16) . . . . ? N61 Sc1 N1 C11 102.31(16) . . . . ? O3 Sc1 N1 C11 -78.8(2) . . . . ? Si3 Sc1 N1 C11 72.89(16) . . . . ? Si4A Sc1 N1 C11 129.80(15) . . . . ? O2 Sc1 N1 C15 11.36(16) . . . . ? O1 Sc1 N1 C15 138.79(16) . . . . ? N61 Sc1 N1 C15 -103.80(17) . . . . ? O3 Sc1 N1 C15 75.1(2) . . . . ? Si3 Sc1 N1 C15 -133.22(15) . . . . ? Si4A Sc1 N1 C15 -76.31(16) . . . . ? O2 Sc1 O1 C2 130.52(14) . . . . ? N61 Sc1 O1 C2 -46.88(17) . . . . ? O3 Sc1 O1 C2 -145.56(15) . . . . ? N1 Sc1 O1 C2 55.38(15) . . . . ? Si3 Sc1 O1 C2 -46.75(14) . . . . ? Si4A Sc1 O1 C2 -43.01(19) . . . . ? Sc1 O1 C2 C1 -50.7(2) . . . . ? Sc1 O1 C2 C3 129.89(17) . . . . ? O1 C2 C3 C4 -174.9(2) . . . . ? C1 C2 C3 C4 5.7(3) . . . . ? O1 C2 C3 Si1 5.5(3) . . . . ? C1 C2 C3 Si1 -173.95(17) . . . . ? C2 C3 C4 C10 1.4(3) . . . . ? Si1 C3 C4 C10 -178.98(18) . . . . ? C3 C4 C10 C5 174.5(2) . . . . ? C3 C4 C10 C9 -4.6(3) . . . . ? C4 C10 C5 C6 -177.8(2) . . . . ? C9 C10 C5 C6 1.3(4) . . . . ? C10 C5 C6 C7 0.1(4) . . . . ? C5 C6 C7 C8 -1.2(4) . . . . ? C6 C7 C8 C9 0.8(4) . . . . ? C7 C8 C9 C10 0.7(3) . . . . ? C7 C8 C9 C1 177.0(2) . . . . ? C5 C10 C9 C8 -1.7(3) . . . . ? C4 C10 C9 C8 177.5(2) . . . . ? C5 C10 C9 C1 -178.2(2) . . . . ? C4 C10 C9 C1 0.9(3) . . . . ? O1 C2 C1 C9 171.24(19) . . . . ? C3 C2 C1 C9 -9.3(3) . . . . ? O1 C2 C1 C11 -12.4(3) . . . . ? C3 C2 C1 C11 167.0(2) . . . . ? C8 C9 C1 C2 -170.4(2) . . . . ? C10 C9 C1 C2 5.9(3) . . . . ? C8 C9 C1 C11 13.2(3) . . . . ? C10 C9 C1 C11 -170.5(2) . . . . ? C15 N1 C11 C12 -4.7(3) . . . . ? Sc1 N1 C11 C12 149.19(17) . . . . ? C15 N1 C11 C1 176.61(19) . . . . ? Sc1 N1 C11 C1 -29.5(3) . . . . ? C2 C1 C11 N1 55.0(3) . . . . ? C9 C1 C11 N1 -128.6(2) . . . . ? C2 C1 C11 C12 -123.7(2) . . . . ? C9 C1 C11 C12 52.7(3) . . . . ? N1 C11 C12 C13 -0.3(3) . . . . ? C1 C11 C12 C13 178.4(2) . . . . ? C11 C12 C13 C14 3.9(4) . . . . ? C4 C3 Si1 C42 135.00(19) . . . . ? C2 C3 Si1 C42 -45.4(2) . . . . ? C4 C3 Si1 C41 18.2(2) . . . . ? C2 C3 Si1 C41 -162.15(19) . . . . ? C4 C3 Si1 C43A -100.1(2) . . . . ? C2 C3 Si1 C43A 79.5(2) . . . . ? C42 Si1 C43A C46A 45.2(3) . . . . ? C41 Si1 C43A C46A 161.5(3) . . . . ? C3 Si1 C43A C46A -80.5(3) . . . . ? C42 Si1 C43A C44A 170.0(3) . . . . ? C41 Si1 C43A C44A -73.8(3) . . . . ? C3 Si1 C43A C44A 44.3(3) . . . . ? C42 Si1 C43A C45A -72.8(3) . . . . ? C41 Si1 C43A C45A 43.4(3) . . . . ? C3 Si1 C43A C45A 161.4(3) . . . . ? O1 Sc1 O2 C22 -127.05(16) . . . . ? N61 Sc1 O2 C22 50.39(18) . . . . ? O3 Sc1 O2 C22 149.38(16) . . . . ? N1 Sc1 O2 C22 -51.56(16) . . . . ? Si3 Sc1 O2 C22 48.2(2) . . . . ? Si4A Sc1 O2 C22 49.26(16) . . . . ? Sc1 O2 C22 C21 48.3(3) . . . . ? Sc1 O2 C22 C23 -133.50(17) . . . . ? O2 C22 C23 C24 175.92(19) . . . . ? C21 C22 C23 C24 -5.9(3) . . . . ? O2 C22 C23 Si2 -8.6(3) . . . . ? C21 C22 C23 Si2 169.52(17) . . . . ? C22 C23 C24 C30 0.1(3) . . . . ? Si2 C23 C24 C30 -175.58(17) . . . . ? C23 C24 C30 C25 -178.7(2) . . . . ? C23 C24 C30 C29 2.9(3) . . . . ? C24 C30 C25 C26 -179.3(2) . . . . ? C29 C30 C25 C26 -0.9(3) . . . . ? C30 C25 C26 C27 -1.9(4) . . . . ? C25 C26 C27 C28 2.2(4) . . . . ? C26 C27 C28 C29 0.2(4) . . . . ? C27 C28 C29 C30 -2.9(3) . . . . ? C27 C28 C29 C21 179.0(2) . . . . ? C25 C30 C29 C28 3.2(3) . . . . ? C24 C30 C29 C28 -178.4(2) . . . . ? C25 C30 C29 C21 -178.6(2) . . . . ? C24 C30 C29 C21 -0.2(3) . . . . ? O2 C22 C21 C29 -173.17(19) . . . . ? C23 C22 C21 C29 8.7(3) . . . . ? O2 C22 C21 C15 11.9(3) . . . . ? C23 C22 C21 C15 -166.3(2) . . . . ? C28 C29 C21 C22 172.5(2) . . . . ? C30 C29 C21 C22 -5.5(3) . . . . ? C28 C29 C21 C15 -12.5(3) . . . . ? C30 C29 C21 C15 169.4(2) . . . . ? C11 N1 C15 C14 6.2(3) . . . . ? Sc1 N1 C15 C14 -147.40(18) . . . . ? C11 N1 C15 C21 -175.8(2) . . . . ? Sc1 N1 C15 C21 30.7(3) . . . . ? C22 C21 C15 N1 -52.4(3) . . . . ? C29 C21 C15 N1 132.6(2) . . . . ? C22 C21 C15 C14 125.7(2) . . . . ? C29 C21 C15 C14 -49.3(3) . . . . ? C12 C13 C14 C15 -2.5(4) . . . . ? N1 C15 C14 C13 -2.6(3) . . . . ? C21 C15 C14 C13 179.3(2) . . . . ? C24 C23 Si2 C52 -139.39(18) . . . . ? C22 C23 Si2 C52 45.2(2) . . . . ? C24 C23 Si2 C51 -20.4(2) . . . . ? C22 C23 Si2 C51 164.17(18) . . . . ? C24 C23 Si2 C53 97.93(19) . . . . ? C22 C23 Si2 C53 -77.5(2) . . . . ? C52 Si2 C53 C54 171.8(2) . . . . ? C51 Si2 C53 C54 52.7(2) . . . . ? C23 Si2 C53 C54 -65.5(2) . . . . ? C52 Si2 C53 C56 -69.9(2) . . . . ? C51 Si2 C53 C56 171.0(2) . . . . ? C23 Si2 C53 C56 52.8(2) . . . . ? C52 Si2 C53 C55 51.2(3) . . . . ? C51 Si2 C53 C55 -67.9(3) . . . . ? C23 Si2 C53 C55 173.9(2) . . . . ? O2 Sc1 N61 Si4A -2.50(16) . . . . ? O1 Sc1 N61 Si4A 175.14(11) . . . . ? O3 Sc1 N61 Si4A -93.89(13) . . . . ? N1 Sc1 N61 Si4A 85.68(13) . . . . ? Si3 Sc1 N61 Si4A 174.9(2) . . . . ? O2 Sc1 N61 Si3 -177.37(9) . . . . ? O1 Sc1 N61 Si3 0.27(15) . . . . ? O3 Sc1 N61 Si3 91.24(12) . . . . ? N1 Sc1 N61 Si3 -89.19(12) . . . . ? Si4A Sc1 N61 Si3 -174.9(2) . . . . ? Si3 N61 Si4A C4B1 -31.9(3) . . . . ? Sc1 N61 Si4A C4B1 153.6(3) . . . . ? Si3 N61 Si4A C4A1 87.3(2) . . . . ? Sc1 N61 Si4A C4A1 -87.2(2) . . . . ? Si3 N61 Si4A Sc1 174.5(2) . . . . ? O2 Sc1 Si4A N61 177.76(14) . . . . ? O1 Sc1 Si4A N61 -7.51(17) . . . . ? O3 Sc1 Si4A N61 90.82(14) . . . . ? N1 Sc1 Si4A N61 -100.32(14) . . . . ? Si3 Sc1 Si4A N61 -2.98(13) . . . . ? O2 Sc1 Si4A C4B1 133.6(4) . . . . ? O1 Sc1 Si4A C4B1 -51.7(4) . . . . ? N61 Sc1 Si4A C4B1 -44.2(4) . . . . ? O3 Sc1 Si4A C4B1 46.6(4) . . . . ? N1 Sc1 Si4A C4B1 -144.5(4) . . . . ? Si3 Sc1 Si4A C4B1 -47.2(4) . . . . ? O2 Sc1 Si4A C4A1 -79.36(17) . . . . ? O1 Sc1 Si4A C4A1 95.37(18) . . . . ? N61 Sc1 Si4A C4A1 102.9(2) . . . . ? O3 Sc1 Si4A C4A1 -166.30(17) . . . . ? N1 Sc1 Si4A C4A1 2.56(17) . . . . ? Si3 Sc1 Si4A C4A1 99.90(16) . . . . ? Si4A N61 Si3 C3A -69.27(18) . . . . ? Sc1 N61 Si3 C3A 105.40(14) . . . . ? Si4A N61 Si3 C3B 58.0(2) . . . . ? Sc1 N61 Si3 C3B -127.30(14) . . . . ? Si4A N61 Si3 Sc1 -174.7(2) . . . . ? O2 Sc1 Si3 N61 4.11(15) . . . . ? O1 Sc1 Si3 N61 -179.76(13) . . . . ? O3 Sc1 Si3 N61 -93.44(13) . . . . ? N1 Sc1 Si3 N61 97.59(13) . . . . ? Si4A Sc1 Si3 N61 2.82(12) . . . . ? O2 Sc1 Si3 C3A -87.30(14) . . . . ? O1 Sc1 Si3 C3A 88.83(12) . . . . ? N61 Sc1 Si3 C3A -91.41(16) . . . . ? O3 Sc1 Si3 C3A 175.16(12) . . . . ? N1 Sc1 Si3 C3A 6.18(12) . . . . ? Si4A Sc1 Si3 C3A -88.58(11) . . . . ? O2 Sc1 Si3 C3B 78.11(16) . . . . ? O1 Sc1 Si3 C3B -105.76(15) . . . . ? N61 Sc1 Si3 C3B 74.00(18) . . . . ? O3 Sc1 Si3 C3B -19.44(15) . . . . ? N1 Sc1 Si3 C3B 171.59(15) . . . . ? Si4A Sc1 Si3 C3B 76.82(14) . . . . ? C106 C101 C102 C103 0.4(4) . . . . ? C101 C102 C103 C104 -0.5(4) . . . . ? C102 C103 C104 C105 0.5(4) . . . . ? C103 C104 C105 C106 -0.4(4) . . . . ? C104 C105 C106 C101 0.4(4) . . . . ? C102 C101 C106 C105 -0.4(4) . . . . ? C116 C111 C112 C113 -0.4(4) . . . . ? C111 C112 C113 C114 -0.1(5) . . . . ? C112 C113 C114 C115 0.4(5) . . . . ? C113 C114 C115 C116 -0.1(5) . . . . ? C114 C115 C116 C111 -0.4(5) . . . . ? C112 C111 C116 C115 0.6(4) . . . . ? C121 C122 C123 C121 0.1(5) . . . 3_656 ? C123 C122 C121 C123 -0.1(5) . . . 3_656 ? #===END data_complex5 _database_code_depnum_ccdc_archive 'CCDC 752789' #TrackingRef 'Cif_files_B920283H.cif' _audit_creation_date 2009-02-05T16:48:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C45 H65 N2 O3 Si4 Y, 2.5(C6 H6)' _chemical_formula_sum 'C60 H80 N2 O3 Si4 Y' _chemical_formula_weight 1078.53 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2947(9) _cell_length_b 23.4235(17) _cell_length_c 22.7434(17) _cell_angle_alpha 90 _cell_angle_beta 93.324(4) _cell_angle_gamma 90 _cell_volume 6006.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6778 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 27.34 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2292 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.623 _exptl_absorpt_correction_T_max 0.795 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_unetI/netI 0.0623 _diffrn_reflns_number 52124 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 13601 _reflns_number_gt 9966 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART, 2006' _computing_cell_refinement 'Bruker SMART, 2006' _computing_data_reduction 'Bruker SAINT, 2006' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0332P)^2^+5.0142P] 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_number_reflns 13601 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0981 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.731 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.066 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.034540(19) 0.175381(9) 0.802846(9) 0.01461(6) Uani 1 1 d . . . N1 N -0.0857(2) 0.19558(10) 0.72554(11) 0.0393(6) Uani 0.5 1 d P A . N1A N -0.0857(2) 0.19558(10) 0.72554(11) 0.0393(6) Uani 0.25 1 d P A 1 Si4A Si -0.2092(2) 0.24443(13) 0.73786(11) 0.0382(5) Uani 0.5 1 d P A 1 H4A H -0.168(7) 0.282(4) 0.781(4) 0.05 Uiso 0.5 1 d P B 1 C4A C -0.3420(5) 0.2111(4) 0.7640(3) 0.059 Uani 0.5 1 d P A 1 H4A3 H -0.3219 0.191 0.8011 0.089 Uiso 0.5 1 calc PR A 1 H4A1 H -0.3738 0.1838 0.7345 0.089 Uiso 0.5 1 calc PR A 1 H4A2 H -0.4016 0.2404 0.7705 0.089 Uiso 0.5 1 calc PR A 1 C5A C -0.2485(7) 0.2824(3) 0.6666(3) 0.053(2) Uani 0.5 1 d P A 1 H5A3 H -0.1774 0.3006 0.6524 0.08 Uiso 0.5 1 calc PR A 1 H5A1 H -0.3086 0.3115 0.673 0.08 Uiso 0.5 1 calc PR A 1 H5A2 H -0.2799 0.2548 0.6373 0.08 Uiso 0.5 1 calc PR A 1 N1B N -0.0857(2) 0.19558(10) 0.72554(11) 0.0393(6) Uani 0.25 1 d P A 2 Si4B Si -0.1671(2) 0.25039(13) 0.71930(11) 0.0382(5) Uani 0.5 1 d P A 2 H4B H -0.140(7) 0.287(4) 0.771(4) 0.05 Uiso 0.5 1 d P C 2 C4B C -0.3241(7) 0.2344(4) 0.7112(6) 0.121 Uani 0.5 1 d P A 2 H4BA H -0.3441 0.2063 0.741 0.182 Uiso 0.5 1 calc PR A 2 H4B3 H -0.3433 0.2188 0.6718 0.182 Uiso 0.5 1 calc PR A 2 H4B2 H -0.3698 0.2694 0.7165 0.182 Uiso 0.5 1 calc PR A 2 C5B C -0.1297(13) 0.3038(4) 0.6620(4) 0.121(5) Uani 0.5 1 d P A 2 H5B3 H -0.0446 0.3122 0.6657 0.181 Uiso 0.5 1 calc PR A 2 H5B1 H -0.1747 0.339 0.6675 0.181 Uiso 0.5 1 calc PR A 2 H5B2 H -0.1503 0.2882 0.6227 0.181 Uiso 0.5 1 calc PR A 2 Si3 Si -0.06522(7) 0.14983(4) 0.66868(4) 0.0395(2) Uani 1 1 d . A . H2 H 0.037(3) 0.1187(12) 0.6866(12) 0.05 Uiso 1 1 d . . . C3A C -0.1864(3) 0.09662(13) 0.65614(12) 0.04 Uani 1 1 d . . . H3C H -0.1943 0.0741 0.692 0.061 Uiso 1 1 calc R A . H3A H -0.1677 0.0712 0.6238 0.061 Uiso 1 1 calc R . . H3B H -0.2612 0.1165 0.646 0.061 Uiso 1 1 calc R . . C3B C -0.0318(3) 0.18361(17) 0.59709(16) 0.0675(12) Uani 1 1 d . . . H3F H -0.0995 0.2069 0.5827 0.101 Uiso 1 1 calc R A . H3D H -0.017 0.1538 0.5682 0.101 Uiso 1 1 calc R . . H3E H 0.0386 0.2079 0.6028 0.101 Uiso 1 1 calc R . . O2 O 0.01131(13) 0.22248(6) 0.88267(7) 0.0182(3) Uani 1 1 d . A . O1 O 0.15553(13) 0.10331(6) 0.80582(6) 0.0165(3) Uani 1 1 d . A . O3 O 0.19806(14) 0.23277(6) 0.78760(7) 0.0191(3) Uani 1 1 d . A . C31 C 0.2966(2) 0.23066(11) 0.83221(11) 0.0252(5) Uani 1 1 d . . . H31A H 0.3398 0.194 0.8301 0.03 Uiso 1 1 calc R A . H31B H 0.2673 0.2348 0.8722 0.03 Uiso 1 1 calc R . . C32 C 0.3748(3) 0.27929(18) 0.81840(17) 0.0753(14) Uani 1 1 d . A . H32B H 0.3595 0.3123 0.8441 0.09 Uiso 1 1 calc R . . H32A H 0.4592 0.2682 0.8247 0.09 Uiso 1 1 calc R . . C33 C 0.3479(3) 0.29396(16) 0.75730(14) 0.0540(9) Uani 1 1 d . . . H33B H 0.4046 0.2751 0.732 0.065 Uiso 1 1 calc R A . H33A H 0.3537 0.3358 0.7518 0.065 Uiso 1 1 calc R . . C34 C 0.2246(2) 0.27407(10) 0.74138(11) 0.0241(5) Uani 1 1 d . A . H34A H 0.1682 0.3064 0.7409 0.029 Uiso 1 1 calc R . . H34B H 0.22 0.2556 0.7021 0.029 Uiso 1 1 calc R . . N999 N -0.07895(16) 0.10766(7) 0.85845(8) 0.0156(4) Uani 1 1 d . A . C15 C -0.13187(19) 0.12669(9) 0.90727(10) 0.0164(5) Uani 1 1 d . . . C21 C -0.1745(2) 0.18671(9) 0.90996(10) 0.0175(5) Uani 1 1 d . A . C29 C -0.2940(2) 0.19756(10) 0.92642(10) 0.0190(5) Uani 1 1 d . . . C28 C -0.3814(2) 0.15403(10) 0.92992(10) 0.0229(5) Uani 1 1 d . A . H28 H -0.3621 0.1158 0.9204 0.027 Uiso 1 1 calc R . . C27 C -0.4933(2) 0.16668(11) 0.94694(11) 0.0249(6) Uani 1 1 d . . . H27 H -0.5503 0.137 0.949 0.03 Uiso 1 1 calc R A . C26 C -0.5246(2) 0.22290(11) 0.96127(10) 0.0250(6) Uani 1 1 d . A . H26 H -0.6013 0.231 0.9741 0.03 Uiso 1 1 calc R . . C25 C -0.4436(2) 0.26579(11) 0.95655(10) 0.0229(5) Uani 1 1 d . . . H25 H -0.4655 0.3039 0.9654 0.027 Uiso 1 1 calc R A . C30 C -0.3277(2) 0.25461(10) 0.93878(10) 0.0187(5) Uani 1 1 d . A . C24 C -0.2425(2) 0.29875(10) 0.93436(10) 0.0198(5) Uani 1 1 d . . . H30 H -0.2648 0.3366 0.9441 0.024 Uiso 1 1 calc R A . C23 C -0.1298(2) 0.28977(9) 0.91680(10) 0.0173(5) Uani 1 1 d . A . C22 C -0.0967(2) 0.23191(9) 0.90243(10) 0.0171(5) Uani 1 1 d . . . Si2 Si -0.02186(6) 0.35135(3) 0.91702(3) 0.01980(14) Uani 1 1 d . . . C51 C 0.0640(3) 0.35117(12) 0.84959(13) 0.0281(6) Uani 1 1 d . A . C52 C -0.1086(2) 0.41974(10) 0.91768(12) 0.0304(6) Uani 1 1 d . A . H52A H -0.054 0.4522 0.917 0.046 Uiso 1 1 calc R . . H52B H -0.1528 0.4215 0.9535 0.046 Uiso 1 1 calc R . . H52C H -0.1641 0.4212 0.883 0.046 Uiso 1 1 calc R . . C53 C 0.0814(2) 0.34837(11) 0.98611(11) 0.0281(6) Uani 1 1 d . A . C54 C 0.1752(3) 0.39562(16) 0.98425(15) 0.0642(11) Uani 1 1 d . . . H54C H 0.1359 0.4329 0.9819 0.096 Uiso 1 1 calc R A . H54A H 0.2218 0.3902 0.9497 0.096 Uiso 1 1 calc R . . H54B H 0.2278 0.3939 1.02 0.096 Uiso 1 1 calc R . . C55 C 0.0100(3) 0.35699(15) 1.04070(12) 0.0475(8) Uani 1 1 d . . . H55C H -0.0535 0.3285 1.0409 0.071 Uiso 1 1 calc R A . H55B H -0.0247 0.3954 1.0398 0.071 Uiso 1 1 calc R . . H55A H 0.0624 0.3527 1.0763 0.071 Uiso 1 1 calc R . . C56 C 0.1435(3) 0.29048(14) 0.99241(14) 0.0514(9) Uani 1 1 d . . . H56C H 0.1903 0.2891 1.03 0.077 Uiso 1 1 calc R A . H56B H 0.1959 0.2853 0.96 0.077 Uiso 1 1 calc R . . H56A H 0.0839 0.26 0.9913 0.077 Uiso 1 1 calc R . . C14 C -0.1449(2) 0.09078(10) 0.95538(10) 0.0205(5) Uani 1 1 d . A . H14 H -0.1801 0.1048 0.9895 0.025 Uiso 1 1 calc R . . C13 C -0.1066(2) 0.03471(10) 0.95334(10) 0.0224(5) Uani 1 1 d . . . H13 H -0.1135 0.0101 0.9862 0.027 Uiso 1 1 calc R A . C11 C -0.04437(19) 0.05201(9) 0.85576(10) 0.0152(5) Uani 1 1 d . . . C1 C 0.00851(19) 0.03035(9) 0.80153(10) 0.0163(5) Uani 1 1 d . A . C9 C -0.0443(2) -0.01805(9) 0.77150(10) 0.0175(5) Uani 1 1 d . . . C8 C -0.1569(2) -0.04092(9) 0.78365(11) 0.0215(5) Uani 1 1 d . A . H8 H -0.1996 -0.0247 0.8143 0.026 Uiso 1 1 calc R . . C7 C -0.2051(2) -0.08591(10) 0.75195(11) 0.0254(5) Uani 1 1 d . . . H7 H -0.2807 -0.1002 0.7608 0.031 Uiso 1 1 calc R A . C6 C -0.1442(2) -0.11123(10) 0.70653(11) 0.0274(6) Uani 1 1 d . A . H6 H -0.1778 -0.1428 0.6852 0.033 Uiso 1 1 calc R . . C5 C -0.0367(2) -0.09014(9) 0.69330(11) 0.0247(5) Uani 1 1 d . . . H5 H 0.0042 -0.1072 0.6625 0.03 Uiso 1 1 calc R A . C10 C 0.0157(2) -0.04332(9) 0.72450(10) 0.0198(5) Uani 1 1 d . A . C4 C 0.1267(2) -0.02042(10) 0.71013(10) 0.0218(5) Uani 1 1 d . . . H4 H 0.1689 -0.0392 0.6808 0.026 Uiso 1 1 calc R A . C3 C 0.1766(2) 0.02738(9) 0.73636(10) 0.0188(5) Uani 1 1 d . A . C2 C 0.1133(2) 0.05464(9) 0.78233(10) 0.0161(5) Uani 1 1 d . A . Si1 Si 0.32325(6) 0.05470(3) 0.71139(3) 0.02184(15) Uani 1 1 d . . . C41 C 0.3497(2) 0.02034(11) 0.63890(11) 0.0315(6) Uani 1 1 d . A . H41A H 0.2833 0.0289 0.6107 0.047 Uiso 1 1 calc R . . H41B H 0.3564 -0.0211 0.6441 0.047 Uiso 1 1 calc R . . H41C H 0.4233 0.0352 0.624 0.047 Uiso 1 1 calc R . . C42 C 0.3224(2) 0.13343(10) 0.69721(12) 0.0307(6) Uani 1 1 d . A . H42A H 0.3969 0.1446 0.6803 0.046 Uiso 1 1 calc R . . H42B H 0.3142 0.1539 0.7343 0.046 Uiso 1 1 calc R . . H42C H 0.2556 0.143 0.6695 0.046 Uiso 1 1 calc R . . C43 C 0.4487(2) 0.03403(11) 0.76677(12) 0.0287(6) Uani 1 1 d . A . C45A C 0.4751(6) -0.0318(3) 0.7667(3) 0.0432(9) Uani 0.5 1 d P A 1 H45B H 0.529 -0.0414 0.8006 0.065 Uiso 0.5 1 calc PR A 1 H45A H 0.512 -0.0421 0.7302 0.065 Uiso 0.5 1 calc PR A 1 H45C H 0.4007 -0.053 0.7692 0.065 Uiso 0.5 1 calc PR A 1 C46A C 0.5672(5) 0.0646(3) 0.7587(3) 0.0432(9) Uani 0.5 1 d P A 1 H46B H 0.6298 0.0465 0.7839 0.065 Uiso 0.5 1 calc PR A 1 H46C H 0.5602 0.1048 0.7696 0.065 Uiso 0.5 1 calc PR A 1 H46A H 0.5872 0.0617 0.7174 0.065 Uiso 0.5 1 calc PR A 1 C44A C 0.4189(6) 0.0456(3) 0.8333(3) 0.0432(9) Uani 0.5 1 d P A 1 H44C H 0.3514 0.0219 0.8433 0.065 Uiso 0.5 1 calc PR A 1 H44B H 0.3991 0.086 0.8382 0.065 Uiso 0.5 1 calc PR A 1 H44A H 0.4881 0.0359 0.8595 0.065 Uiso 0.5 1 calc PR A 1 C45B C 0.4288(5) -0.0267(3) 0.7852(3) 0.0324(8) Uani 0.5 1 d P A 2 H45D H 0.4959 -0.0394 0.8112 0.049 Uiso 0.5 1 calc PR A 2 H45E H 0.4219 -0.0511 0.7502 0.049 Uiso 0.5 1 calc PR A 2 H45F H 0.3556 -0.029 0.8062 0.049 Uiso 0.5 1 calc PR A 2 C46B C 0.5641(5) 0.0385(3) 0.7323(3) 0.0324(8) Uani 0.5 1 d P A 2 H46E H 0.6334 0.0314 0.7592 0.049 Uiso 0.5 1 calc PR A 2 H46F H 0.5697 0.0769 0.7154 0.049 Uiso 0.5 1 calc PR A 2 H46D H 0.5615 0.0102 0.7006 0.049 Uiso 0.5 1 calc PR A 2 C44B C 0.4525(5) 0.0753(3) 0.8159(2) 0.0324(8) Uani 0.5 1 d P A 2 H44F H 0.3759 0.0755 0.834 0.049 Uiso 0.5 1 calc PR A 2 44DE H 0.469 0.1135 0.8009 0.049 Uiso 0.5 1 calc PR A 2 H44D H 0.5151 0.0643 0.8453 0.049 Uiso 0.5 1 calc PR A 2 C12 C -0.0582(2) 0.01510(9) 0.90261(10) 0.0201(5) Uani 1 1 d . A . H12 H -0.0343 -0.0237 0.8999 0.024 Uiso 1 1 calc R . . H51A H 0.010(2) 0.3538(11) 0.8148(12) 0.03 Uiso 1 1 d . . . H51B H 0.107(2) 0.3183(12) 0.8477(11) 0.03 Uiso 1 1 d . . . H51C H 0.118(2) 0.3834(12) 0.8473(11) 0.03 Uiso 1 1 d . . . C101 C 0.3194(3) 0.08231(17) 0.06161(15) 0.0544(9) Uani 1 1 d . . . H101 H 0.3465 0.088 0.1015 0.065 Uiso 1 1 calc R . . C102 C 0.3635(3) 0.03786(15) 0.03020(15) 0.0503(9) Uani 1 1 d . . . H102 H 0.4207 0.0127 0.0482 0.06 Uiso 1 1 calc R . . C103 C 0.3239(3) 0.03008(14) -0.02777(15) 0.0458(8) Uani 1 1 d . . . H103 H 0.354 -0.0005 -0.05 0.055 Uiso 1 1 calc R . . C104 C 0.2398(2) 0.06705(15) -0.05364(14) 0.0444(8) Uani 1 1 d . . . H104 H 0.2127 0.0617 -0.0936 0.053 Uiso 1 1 calc R . . C105 C 0.1958(3) 0.11109(15) -0.02182(15) 0.0452(8) Uani 1 1 d . . . H105 H 0.1378 0.136 -0.0396 0.054 Uiso 1 1 calc R . . C106 C 0.2355(3) 0.11909(16) 0.03548(15) 0.0525(9) Uani 1 1 d . . . H106 H 0.2056 0.1499 0.0575 0.063 Uiso 1 1 calc R . . C111 C 0.8266(3) 0.10339(11) 0.13311(12) 0.0350(7) Uani 1 1 d . . . H111 H 0.8311 0.0675 0.1526 0.042 Uiso 1 1 calc R . . C112 C 0.9283(3) 0.13495(11) 0.12664(12) 0.0337(6) Uani 1 1 d . . . H112 H 1.0029 0.1209 0.1418 0.04 Uiso 1 1 calc R . . C113 C 0.9214(3) 0.18716(12) 0.09804(12) 0.0383(7) Uani 1 1 d . . . H113 H 0.9912 0.209 0.0937 0.046 Uiso 1 1 calc R . . C114 C 0.8137(3) 0.20745(12) 0.07600(12) 0.0417(8) Uani 1 1 d . . . H114 H 0.8096 0.2432 0.0562 0.05 Uiso 1 1 calc R . . C115 C 0.7116(3) 0.17647(12) 0.08225(11) 0.0384(7) Uani 1 1 d . . . H115 H 0.6373 0.1908 0.0669 0.046 Uiso 1 1 calc R . . C116 C 0.7178(3) 0.12416(12) 0.11112(11) 0.0351(7) Uani 1 1 d . . . H116 H 0.6477 0.1026 0.1158 0.042 Uiso 1 1 calc R . . C121 C -0.0629(3) -0.02065(18) 0.54552(14) 0.0588(10) Uani 1 1 d . . . H121 H -0.1063 -0.035 0.5769 0.071 Uiso 1 1 calc R . . C122 C 0.0260(3) 0.01837(18) 0.55681(14) 0.0599(10) Uani 1 1 d . . . H122 H 0.044 0.0311 0.596 0.072 Uiso 1 1 calc R . . C123 C 0.0895(3) 0.03914(18) 0.51123(15) 0.0609(10) Uani 1 1 d . . . H123 H 0.1512 0.0661 0.519 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.01429(11) 0.01337(10) 0.01646(11) 0.00234(9) 0.00335(8) 0.00009(9) N1 0.0334(14) 0.0384(13) 0.0443(15) 0.0202(11) -0.0147(11) -0.0112(11) N1A 0.0334(14) 0.0384(13) 0.0443(15) 0.0202(11) -0.0147(11) -0.0112(11) Si4A 0.0426(15) 0.0360(7) 0.0337(13) -0.0014(9) -0.0165(8) 0.0069(10) C4A 0.016 0.114 0.047 -0.033 -0.003 0.016 C5A 0.079(5) 0.033(3) 0.043(4) -0.006(3) -0.035(4) 0.021(4) N1B 0.0334(14) 0.0384(13) 0.0443(15) 0.0202(11) -0.0147(11) -0.0112(11) Si4B 0.0426(15) 0.0360(7) 0.0337(13) -0.0014(9) -0.0165(8) 0.0069(10) C4B 0.047 0.093 0.219 -0.075 -0.039 0.038 C5B 0.263(15) 0.045(5) 0.060(6) 0.028(4) 0.048(8) 0.060(7) Si3 0.0220(4) 0.0600(5) 0.0361(5) 0.0290(4) -0.0015(3) -0.0031(4) C3A 0.034 0.059 0.03 0 0.004 0.001 C3B 0.056(2) 0.094(3) 0.054(2) 0.048(2) 0.0153(18) 0.008(2) O2 0.0161(8) 0.0161(7) 0.0231(9) -0.0008(6) 0.0064(7) -0.0014(6) O1 0.0157(8) 0.0159(7) 0.0182(8) 0.0007(6) 0.0040(6) -0.0007(6) O3 0.0193(9) 0.0190(8) 0.0190(8) 0.0045(7) 0.0018(7) -0.0033(7) C31 0.0219(13) 0.0288(13) 0.0245(13) 0.0034(11) -0.0011(11) -0.0030(11) C32 0.056(2) 0.098(3) 0.068(3) 0.047(2) -0.029(2) -0.053(2) C33 0.0422(19) 0.071(2) 0.047(2) 0.0282(17) -0.0066(16) -0.0328(17) C34 0.0284(14) 0.0223(12) 0.0221(13) 0.0083(10) 0.0063(11) -0.0017(11) N999 0.0136(10) 0.0164(9) 0.0169(10) 0.0008(8) 0.0030(8) -0.0010(7) C15 0.0123(11) 0.0169(10) 0.0204(12) 0.0000(9) 0.0032(9) -0.0041(9) C21 0.0177(12) 0.0186(11) 0.0164(11) -0.0029(9) 0.0031(9) -0.0022(9) C29 0.0170(12) 0.0240(11) 0.0164(12) -0.0022(9) 0.0029(10) -0.0002(10) C28 0.0206(13) 0.0253(12) 0.0231(13) -0.0048(10) 0.0041(10) -0.0022(10) C27 0.0188(13) 0.0334(14) 0.0230(13) -0.0024(11) 0.0044(10) -0.0083(11) C26 0.0156(12) 0.0385(14) 0.0211(13) -0.0003(11) 0.0038(10) 0.0036(11) C25 0.0216(13) 0.0293(13) 0.0180(12) -0.0032(10) 0.0020(10) 0.0053(11) C30 0.0181(12) 0.0249(12) 0.0131(11) -0.0023(9) 0.0024(9) 0.0019(10) C24 0.0228(13) 0.0180(11) 0.0183(12) -0.0025(9) 0.0000(10) 0.0031(10) C23 0.0193(12) 0.0180(11) 0.0145(11) -0.0008(9) -0.0003(9) 0.0002(9) C22 0.0180(12) 0.0199(11) 0.0133(11) -0.0006(9) 0.0007(9) -0.0004(9) Si2 0.0217(4) 0.0160(3) 0.0218(3) -0.0021(3) 0.0028(3) -0.0017(3) C51 0.0334(16) 0.0200(13) 0.0317(15) 0.0003(11) 0.0101(13) -0.0038(12) C52 0.0312(15) 0.0200(12) 0.0405(16) -0.0023(11) 0.0057(12) -0.0016(11) C53 0.0295(15) 0.0284(13) 0.0259(14) -0.0030(11) -0.0014(11) -0.0038(11) C54 0.062(2) 0.076(3) 0.052(2) 0.0112(19) -0.0233(18) -0.042(2) C55 0.054(2) 0.064(2) 0.0242(15) -0.0089(14) -0.0002(14) 0.0005(17) C56 0.050(2) 0.061(2) 0.0404(19) -0.0078(16) -0.0196(16) 0.0190(17) C14 0.0188(12) 0.0231(12) 0.0204(12) -0.0006(10) 0.0087(10) -0.0038(10) C13 0.0237(13) 0.0228(12) 0.0211(13) 0.0064(10) 0.0053(10) -0.0032(10) C11 0.0124(11) 0.0153(10) 0.0180(12) 0.0018(9) 0.0014(9) -0.0013(9) C1 0.0174(12) 0.0142(10) 0.0175(11) 0.0041(9) 0.0024(10) 0.0045(9) C9 0.0181(12) 0.0131(10) 0.0213(12) 0.0037(9) 0.0002(10) 0.0044(9) C8 0.0197(13) 0.0174(11) 0.0274(13) 0.0020(10) 0.0008(10) 0.0036(10) C7 0.0206(13) 0.0210(12) 0.0342(15) 0.0031(11) -0.0030(11) -0.0013(10) C6 0.0310(15) 0.0196(12) 0.0304(14) -0.0023(10) -0.0084(12) -0.0017(11) C5 0.0331(14) 0.0171(11) 0.0236(13) -0.0014(10) -0.0007(11) 0.0053(11) C10 0.0226(13) 0.0175(11) 0.0191(12) 0.0022(9) -0.0014(10) 0.0058(10) C4 0.0269(14) 0.0185(11) 0.0207(12) 0.0012(9) 0.0064(11) 0.0064(10) C3 0.0207(12) 0.0173(11) 0.0191(12) 0.0042(9) 0.0080(10) 0.0050(9) C2 0.0189(12) 0.0135(10) 0.0158(11) 0.0048(9) 0.0008(9) 0.0033(9) Si1 0.0219(4) 0.0185(3) 0.0263(4) 0.0025(3) 0.0120(3) 0.0035(3) C41 0.0361(16) 0.0299(14) 0.0300(15) 0.0034(11) 0.0153(12) 0.0075(12) C42 0.0282(15) 0.0230(12) 0.0429(16) 0.0051(12) 0.0183(13) 0.0010(11) C43 0.0199(13) 0.0283(13) 0.0388(16) 0.0022(12) 0.0089(12) 0.0032(11) C45A 0.029(2) 0.047(2) 0.053(3) 0.0079(18) -0.0012(18) 0.0090(17) C46A 0.029(2) 0.047(2) 0.053(3) 0.0079(18) -0.0012(18) 0.0090(17) C44A 0.029(2) 0.047(2) 0.053(3) 0.0079(18) -0.0012(18) 0.0090(17) C45B 0.0237(17) 0.0427(19) 0.0302(19) 0.0025(15) -0.0027(14) 0.0087(15) C46B 0.0237(17) 0.0427(19) 0.0302(19) 0.0025(15) -0.0027(14) 0.0087(15) C44B 0.0237(17) 0.0427(19) 0.0302(19) 0.0025(15) -0.0027(14) 0.0087(15) C12 0.0205(13) 0.0146(11) 0.0258(13) 0.0045(9) 0.0049(10) -0.0010(9) C101 0.041(2) 0.083(3) 0.0366(18) 0.0191(18) -0.0144(15) -0.0201(19) C102 0.0310(17) 0.061(2) 0.058(2) 0.0312(18) -0.0064(16) -0.0085(16) C103 0.0322(17) 0.0532(19) 0.052(2) 0.0126(16) 0.0043(15) -0.0163(15) C104 0.0245(16) 0.073(2) 0.0352(17) 0.0235(16) -0.0063(13) -0.0233(16) C105 0.0206(15) 0.061(2) 0.053(2) 0.0257(17) -0.0038(14) -0.0114(15) C106 0.0350(18) 0.068(2) 0.054(2) 0.0071(18) 0.0001(16) -0.0109(17) C111 0.0477(18) 0.0272(14) 0.0301(15) 0.0044(12) 0.0020(13) 0.0102(13) C112 0.0409(17) 0.0324(14) 0.0275(15) -0.0031(12) -0.0009(13) 0.0099(13) C113 0.053(2) 0.0329(15) 0.0287(15) -0.0011(12) 0.0026(14) -0.0004(14) C114 0.071(2) 0.0272(14) 0.0263(15) 0.0019(12) -0.0062(15) 0.0079(15) C115 0.0527(19) 0.0398(16) 0.0219(14) -0.0074(13) -0.0046(13) 0.0225(15) C116 0.0416(17) 0.0372(15) 0.0268(15) -0.0042(12) 0.0039(13) 0.0055(13) C121 0.040(2) 0.103(3) 0.0338(19) 0.0253(19) 0.0100(15) 0.013(2) C122 0.042(2) 0.109(3) 0.0288(17) 0.0110(19) 0.0043(15) 0.012(2) C123 0.046(2) 0.094(3) 0.042(2) 0.0160(19) 0.0035(17) 0.005(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O2 2.1535(15) . ? Y1 O1 2.1705(15) . ? Y1 N1 2.210(2) . ? Y1 O3 2.3264(15) . ? Y1 N999 2.4385(17) . ? Y1 C2 3.009(2) . ? Y1 Si3 3.2465(9) . ? Y1 Si4B 3.374(3) . ? N1 Si4B 1.581(4) . ? N1 Si3 1.706(3) . ? N1 Si4A 1.839(4) . ? Si4A C4A 1.821(7) . ? Si4A C5A 1.878(7) . ? Si4A H4A 1.39(9) . ? Si4A H4B 1.46(9) . ? C4A H4A3 0.98 . ? C4A H4A1 0.98 . ? C4A H4A2 0.98 . ? C5A H5A3 0.98 . ? C5A H5A1 0.98 . ? C5A H5A2 0.98 . ? Si4B C4B 1.811(9) . ? Si4B C5B 1.873(8) . ? Si4B H4A 1.59(9) . ? Si4B H4B 1.49(9) . ? C4B H4BA 0.98 . ? C4B H4B3 0.98 . ? C4B H4B2 0.98 . ? C5B H5B3 0.98 . ? C5B H5B1 0.98 . ? C5B H5B2 0.98 . ? Si3 C3A 1.861(3) . ? Si3 C3B 1.868(3) . ? Si3 H2 1.40(3) . ? C3A H3C 0.98 . ? C3A H3A 0.98 . ? C3A H3B 0.98 . ? C3B H3F 0.98 . ? C3B H3D 0.98 . ? C3B H3E 0.98 . ? O2 C22 1.342(3) . ? O1 C2 1.335(3) . ? O3 C31 1.463(3) . ? O3 C34 1.472(3) . ? C31 C32 1.486(4) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.447(4) . ? C32 H32B 0.99 . ? C32 H32A 0.99 . ? C33 C34 1.493(4) . ? C33 H33B 0.99 . ? C33 H33A 0.99 . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? N999 C11 1.363(3) . ? N999 C15 1.366(3) . ? C15 C14 1.395(3) . ? C15 C21 1.488(3) . ? C21 C22 1.393(3) . ? C21 C29 1.444(3) . ? C29 C30 1.422(3) . ? C29 C28 1.424(3) . ? C28 C27 1.376(3) . ? C28 H28 0.95 . ? C27 C26 1.406(3) . ? C27 H27 0.95 . ? C26 C25 1.367(3) . ? C26 H26 0.95 . ? C25 C30 1.416(3) . ? C25 H25 0.95 . ? C30 C24 1.420(3) . ? C24 C23 1.373(3) . ? C24 H30 0.95 . ? C23 C22 1.448(3) . ? C23 Si2 1.888(2) . ? Si2 C51 1.861(3) . ? Si2 C52 1.878(3) . ? Si2 C53 1.903(3) . ? C51 H51A 0.97(3) . ? C51 H51B 0.91(3) . ? C51 H51C 0.98(3) . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? C53 C56 1.529(4) . ? C53 C55 1.533(4) . ? C53 C54 1.534(4) . ? C54 H54C 0.98 . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C55 H55C 0.98 . ? C55 H55B 0.98 . ? C55 H55A 0.98 . ? C56 H56C 0.98 . ? C56 H56B 0.98 . ? C56 H56A 0.98 . ? C14 C13 1.384(3) . ? C14 H14 0.95 . ? C13 C12 1.384(3) . ? C13 H13 0.95 . ? C11 C12 1.388(3) . ? C11 C1 1.490(3) . ? C1 C2 1.405(3) . ? C1 C9 1.436(3) . ? C9 C8 1.422(3) . ? C9 C10 1.427(3) . ? C8 C7 1.371(3) . ? C8 H8 0.95 . ? C7 C6 1.405(4) . ? C7 H7 0.95 . ? C6 C5 1.361(4) . ? C6 H6 0.95 . ? C5 C10 1.417(3) . ? C5 H5 0.95 . ? C10 C4 1.419(3) . ? C4 C3 1.374(3) . ? C4 H4 0.95 . ? C3 C2 1.449(3) . ? C3 Si1 1.893(2) . ? Si1 C42 1.872(2) . ? Si1 C41 1.874(3) . ? Si1 C43 1.903(3) . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 C44B 1.476(6) . ? C43 C45B 1.503(7) . ? C43 C46A 1.538(7) . ? C43 C46B 1.563(6) . ? C43 C45A 1.571(7) . ? C43 C44A 1.593(7) . ? C45A H45B 0.98 . ? C45A H45A 0.98 . ? C45A H45C 0.98 . ? C46A H46B 0.98 . ? C46A H46C 0.98 . ? C46A H46A 0.98 . ? C44A H44C 0.98 . ? C44A H44B 0.98 . ? C44A H44A 0.98 . ? C45B H45D 0.98 . ? C45B H45E 0.98 . ? C45B H45F 0.98 . ? C46B H46E 0.98 . ? C46B H46F 0.98 . ? C46B H46D 0.98 . ? C44B H44F 0.98 . ? C44B 44DE 0.98 . ? C44B H44D 0.98 . ? C12 H12 0.95 . ? C101 C102 1.373(5) . ? C101 C106 1.389(5) . ? C101 H101 0.95 . ? C102 C103 1.379(5) . ? C102 H102 0.95 . ? C103 C104 1.390(4) . ? C103 H103 0.95 . ? C104 C105 1.370(5) . ? C104 H104 0.95 . ? C105 C106 1.366(5) . ? C105 H105 0.95 . ? C106 H106 0.95 . ? C111 C112 1.382(4) . ? C111 C116 1.387(4) . ? C111 H111 0.95 . ? C112 C113 1.385(4) . ? C112 H112 0.95 . ? C113 C114 1.373(4) . ? C113 H113 0.95 . ? C114 C115 1.377(4) . ? C114 H114 0.95 . ? C115 C116 1.390(4) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C122 1.371(5) . ? C121 C123 1.378(5) 3_556 ? C121 H121 0.95 . ? C122 C123 1.382(4) . ? C122 H122 0.95 . ? C123 C121 1.378(5) 3_556 ? C123 H123 0.95 . ? 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 Y1 O1 118.65(6) . . ? O2 Y1 N1 117.51(8) . . ? O1 Y1 N1 123.24(8) . . ? O2 Y1 O3 88.07(5) . . ? O1 Y1 O3 87.14(5) . . ? N1 Y1 O3 102.37(7) . . ? O2 Y1 N999 78.61(6) . . ? O1 Y1 N999 80.03(6) . . ? N1 Y1 N999 103.57(7) . . ? O3 Y1 N999 154.01(6) . . ? O2 Y1 C2 131.59(6) . . ? O1 Y1 C2 23.46(6) . . ? N1 Y1 C2 104.56(8) . . ? O3 Y1 C2 105.99(6) . . ? N999 Y1 C2 68.78(6) . . ? O2 Y1 Si3 146.53(4) . . ? O1 Y1 Si3 93.98(4) . . ? N1 Y1 Si3 29.28(7) . . ? O3 Y1 Si3 101.64(4) . . ? N999 Y1 Si3 101.73(5) . . ? C2 Y1 Si3 76.74(5) . . ? O2 Y1 Si4B 95.55(6) . . ? O1 Y1 Si4B 145.67(6) . . ? N1 Y1 Si4B 22.58(8) . . ? O3 Y1 Si4B 97.53(6) . . ? N999 Y1 Si4B 105.83(6) . . ? C2 Y1 Si4B 126.73(7) . . ? Si3 Y1 Si4B 51.72(5) . . ? Si4B N1 Si3 123.08(17) . . ? Si3 N1 Si4A 130.09(16) . . ? Si4B N1 Y1 124.95(17) . . ? Si3 N1 Y1 111.39(12) . . ? Si4A N1 Y1 116.67(15) . . ? C4A Si4A N1 115.4(3) . . ? C4A Si4A C5A 109.1(4) . . ? N1 Si4A C5A 107.8(3) . . ? C4A Si4A H4A 107(3) . . ? N1 Si4A H4A 106(4) . . ? C5A Si4A H4A 112(4) . . ? C4A Si4A H4B 123(3) . . ? N1 Si4A H4B 97(3) . . ? C5A Si4A H4B 102(3) . . ? Si4A C4A H4A3 109.5 . . ? Si4A C4A H4A1 109.5 . . ? H4A3 C4A H4A1 109.5 . . ? Si4A C4A H4A2 109.5 . . ? H4A3 C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? Si4A C5A H5A3 109.5 . . ? Si4A C5A H5A1 109.5 . . ? H5A3 C5A H5A1 109.5 . . ? Si4A C5A H5A2 109.5 . . ? H5A3 C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? N1 Si4B C4B 113.7(4) . . ? N1 Si4B C5B 116.9(4) . . ? C4B Si4B C5B 109.1(7) . . ? C4B Si4B Y1 125.0(4) . . ? C5B Si4B Y1 124.6(5) . . ? N1 Si4B H4A 109(3) . . ? C4B Si4B H4A 98(3) . . ? C5B Si4B H4A 108(3) . . ? Y1 Si4B H4A 77(3) . . ? N1 Si4B H4B 108(4) . . ? C4B Si4B H4B 111(3) . . ? C5B Si4B H4B 97(3) . . ? Y1 Si4B H4B 76(4) . . ? Si4B C4B H4BA 109.5 . . ? Si4B C4B H4B3 109.5 . . ? H4BA C4B H4B3 109.5 . . ? Si4B C4B H4B2 109.5 . . ? H4BA C4B H4B2 109.5 . . ? H4B3 C4B H4B2 109.5 . . ? Si4B C5B H5B3 109.5 . . ? Si4B C5B H5B1 109.5 . . ? H5B3 C5B H5B1 109.5 . . ? Si4B C5B H5B2 109.5 . . ? H5B3 C5B H5B2 109.5 . . ? H5B1 C5B H5B2 109.5 . . ? N1 Si3 C3A 113.96(12) . . ? N1 Si3 C3B 115.97(16) . . ? C3A Si3 C3B 109.51(17) . . ? C3A Si3 Y1 118.66(9) . . ? C3B Si3 Y1 131.64(14) . . ? N1 Si3 H2 104.6(12) . . ? C3A Si3 H2 106.4(12) . . ? C3B Si3 H2 105.5(12) . . ? Y1 Si3 H2 65.7(12) . . ? Si3 C3A H3C 109.5 . . ? Si3 C3A H3A 109.5 . . ? H3C C3A H3A 109.5 . . ? Si3 C3A H3B 109.5 . . ? H3C C3A H3B 109.5 . . ? H3A C3A H3B 109.5 . . ? Si3 C3B H3F 109.5 . . ? Si3 C3B H3D 109.5 . . ? H3F C3B H3D 109.5 . . ? Si3 C3B H3E 109.5 . . ? H3F C3B H3E 109.5 . . ? H3D C3B H3E 109.5 . . ? C22 O2 Y1 121.61(13) . . ? C2 O1 Y1 116.22(13) . . ? C31 O3 C34 109.84(17) . . ? C31 O3 Y1 117.11(12) . . ? C34 O3 Y1 133.03(13) . . ? O3 C31 C32 105.4(2) . . ? O3 C31 H31A 110.7 . . ? C32 C31 H31A 110.7 . . ? O3 C31 H31B 110.7 . . ? C32 C31 H31B 110.7 . . ? H31A C31 H31B 108.8 . . ? C33 C32 C31 106.9(3) . . ? C33 C32 H32B 110.3 . . ? C31 C32 H32B 110.3 . . ? C33 C32 H32A 110.3 . . ? C31 C32 H32A 110.3 . . ? H32B C32 H32A 108.6 . . ? C32 C33 C34 107.5(2) . . ? C32 C33 H33B 110.2 . . ? C34 C33 H33B 110.2 . . ? C32 C33 H33A 110.2 . . ? C34 C33 H33A 110.2 . . ? H33B C33 H33A 108.5 . . ? O3 C34 C33 104.9(2) . . ? O3 C34 H34A 110.8 . . ? C33 C34 H34A 110.8 . . ? O3 C34 H34B 110.8 . . ? C33 C34 H34B 110.8 . . ? H34A C34 H34B 108.8 . . ? C11 N999 C15 119.25(18) . . ? C11 N999 Y1 115.98(13) . . ? C15 N999 Y1 118.51(13) . . ? N999 C15 C14 120.8(2) . . ? N999 C15 C21 119.97(19) . . ? C14 C15 C21 119.2(2) . . ? C22 C21 C29 120.3(2) . . ? C22 C21 C15 120.3(2) . . ? C29 C21 C15 119.12(19) . . ? C30 C29 C28 117.9(2) . . ? C30 C29 C21 118.8(2) . . ? C28 C29 C21 123.3(2) . . ? C27 C28 C29 120.8(2) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C27 C26 120.9(2) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C25 C26 C27 119.5(2) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C26 C25 C30 121.3(2) . . ? C26 C25 H25 119.3 . . ? C30 C25 H25 119.3 . . ? C25 C30 C24 121.8(2) . . ? C25 C30 C29 119.5(2) . . ? C24 C30 C29 118.7(2) . . ? C23 C24 C30 123.6(2) . . ? C23 C24 H30 118.2 . . ? C30 C24 H30 118.2 . . ? C24 C23 C22 117.7(2) . . ? C24 C23 Si2 119.45(17) . . ? C22 C23 Si2 122.70(17) . . ? O2 C22 C21 120.55(19) . . ? O2 C22 C23 118.77(19) . . ? C21 C22 C23 120.7(2) . . ? C51 Si2 C52 107.78(13) . . ? C51 Si2 C23 111.28(11) . . ? C52 Si2 C23 108.35(11) . . ? C51 Si2 C53 110.89(13) . . ? C52 Si2 C53 108.64(12) . . ? C23 Si2 C53 109.81(11) . . ? Si2 C51 H51A 110.0(16) . . ? Si2 C51 H51B 110.2(17) . . ? H51A C51 H51B 109(2) . . ? Si2 C51 H51C 113.6(15) . . ? H51A C51 H51C 106(2) . . ? H51B C51 H51C 108(2) . . ? Si2 C52 H52A 109.5 . . ? Si2 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si2 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C56 C53 C55 107.5(2) . . ? C56 C53 C54 109.2(3) . . ? C55 C53 C54 108.9(3) . . ? C56 C53 Si2 111.44(18) . . ? C55 C53 Si2 109.73(19) . . ? C54 C53 Si2 110.00(19) . . ? C53 C54 H54C 109.5 . . ? C53 C54 H54A 109.5 . . ? H54C C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54C C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C55 H55C 109.5 . . ? C53 C55 H55B 109.5 . . ? H55C C55 H55B 109.5 . . ? C53 C55 H55A 109.5 . . ? H55C C55 H55A 109.5 . . ? H55B C55 H55A 109.5 . . ? C53 C56 H56C 109.5 . . ? C53 C56 H56B 109.5 . . ? H56C C56 H56B 109.5 . . ? C53 C56 H56A 109.5 . . ? H56C C56 H56A 109.5 . . ? H56B C56 H56A 109.5 . . ? C13 C14 C15 119.9(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C12 C13 C14 118.8(2) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? N999 C11 C12 121.1(2) . . ? N999 C11 C1 119.49(18) . . ? C12 C11 C1 119.45(19) . . ? C2 C1 C9 120.4(2) . . ? C2 C1 C11 120.3(2) . . ? C9 C1 C11 119.15(19) . . ? C8 C9 C10 117.3(2) . . ? C8 C9 C1 123.8(2) . . ? C10 C9 C1 118.8(2) . . ? C7 C8 C9 121.3(2) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C7 C6 121.0(2) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C5 C6 C7 119.4(2) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C6 C5 C10 121.5(2) . . ? C6 C5 H5 119.3 . . ? C10 C5 H5 119.3 . . ? C5 C10 C4 121.7(2) . . ? C5 C10 C9 119.6(2) . . ? C4 C10 C9 118.7(2) . . ? C3 C4 C10 123.6(2) . . ? C3 C4 H4 118.2 . . ? C10 C4 H4 118.2 . . ? C4 C3 C2 117.7(2) . . ? C4 C3 Si1 119.28(17) . . ? C2 C3 Si1 122.99(17) . . ? O1 C2 C1 120.60(19) . . ? O1 C2 C3 119.0(2) . . ? C1 C2 C3 120.4(2) . . ? C1 C2 Y1 94.04(13) . . ? C3 C2 Y1 133.53(14) . . ? C42 Si1 C41 105.72(12) . . ? C42 Si1 C3 112.88(11) . . ? C41 Si1 C3 107.80(12) . . ? C42 Si1 C43 111.16(12) . . ? C41 Si1 C43 108.81(12) . . ? C3 Si1 C43 110.25(11) . . ? 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 . . ? Si1 C42 H42A 109.5 . . ? Si1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44B C43 C45B 114.0(4) . . ? C44B C43 C46A 78.4(4) . . ? C45B C43 C46A 128.2(4) . . ? C44B C43 C46B 110.3(4) . . ? C45B C43 C46B 110.3(4) . . ? C44B C43 C45A 130.3(4) . . ? C46A C43 C45A 106.8(4) . . ? C46B C43 C45A 84.4(4) . . ? C45B C43 C44A 81.5(4) . . ? C46A C43 C44A 105.5(4) . . ? C46B C43 C44A 133.9(4) . . ? C45A C43 C44A 102.6(4) . . ? C44B C43 Si1 108.8(3) . . ? C45B C43 Si1 107.9(3) . . ? C46A C43 Si1 115.0(3) . . ? C46B C43 Si1 105.1(2) . . ? C45A C43 Si1 112.5(3) . . ? C44A C43 Si1 113.3(3) . . ? C43 C45A H45B 109.5 . . ? C43 C45A H45A 109.5 . . ? C43 C45A H45C 109.5 . . ? C43 C46A H46B 109.5 . . ? C43 C46A H46C 109.5 . . ? C43 C46A H46A 109.5 . . ? C43 C44A H44C 109.5 . . ? C43 C44A H44B 109.5 . . ? C43 C44A H44A 109.5 . . ? C43 C45B H45D 109.5 . . ? C43 C45B H45E 109.5 . . ? H45D C45B H45E 109.5 . . ? C43 C45B H45F 109.5 . . ? H45D C45B H45F 109.5 . . ? H45E C45B H45F 109.5 . . ? C43 C46B H46E 109.5 . . ? C43 C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? C43 C46B H46D 109.5 . . ? H46E C46B H46D 109.5 . . ? H46F C46B H46D 109.5 . . ? C43 C44B H44F 109.5 . . ? C43 C44B 44DE 109.5 . . ? H44F C44B 44DE 109.5 . . ? C43 C44B H44D 109.5 . . ? H44F C44B H44D 109.5 . . ? 44DE C44B H44D 109.5 . . ? C13 C12 C11 120.0(2) . . ? C13 C12 H12 120 . . ? C11 C12 H12 120 . . ? C102 C101 C106 120.5(3) . . ? C102 C101 H101 119.8 . . ? C106 C101 H101 119.8 . . ? C101 C102 C103 119.4(3) . . ? C101 C102 H102 120.3 . . ? C103 C102 H102 120.3 . . ? C102 C103 C104 119.9(3) . . ? C102 C103 H103 120.1 . . ? C104 C103 H103 120.1 . . ? C105 C104 C103 120.3(3) . . ? C105 C104 H104 119.8 . . ? C103 C104 H104 119.8 . . ? C106 C105 C104 119.9(3) . . ? C106 C105 H105 120.1 . . ? C104 C105 H105 120.1 . . ? C105 C106 C101 120.1(4) . . ? C105 C106 H106 120 . . ? C101 C106 H106 120 . . ? C112 C111 C116 119.9(3) . . ? C112 C111 H111 120 . . ? C116 C111 H111 120 . . ? C111 C112 C113 119.8(3) . . ? C111 C112 H112 120.1 . . ? C113 C112 H112 120.1 . . ? C114 C113 C112 120.1(3) . . ? C114 C113 H113 119.9 . . ? C112 C113 H113 119.9 . . ? C113 C114 C115 120.6(3) . . ? C113 C114 H114 119.7 . . ? C115 C114 H114 119.7 . . ? C114 C115 C116 119.6(3) . . ? C114 C115 H115 120.2 . . ? C116 C115 H115 120.2 . . ? C111 C116 C115 119.9(3) . . ? C111 C116 H116 120 . . ? C115 C116 H116 120 . . ? C122 C121 C123 120.2(3) . 3_556 ? C122 C121 H121 119.9 . . ? C123 C121 H121 119.9 3_556 . ? C121 C122 C123 120.0(3) . . ? C121 C122 H122 120 . . ? C123 C122 H122 120 . . ? C121 C123 C122 119.8(4) 3_556 . ? C121 C123 H123 120.1 3_556 . ? C122 C123 H123 120.1 . . ? 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 Y1 N1 Si4B 14.6(2) . . . . ? O1 Y1 N1 Si4B -174.48(15) . . . . ? O3 Y1 N1 Si4B -79.73(18) . . . . ? N999 Y1 N1 Si4B 98.66(18) . . . . ? C2 Y1 N1 Si4B 169.87(17) . . . . ? Si3 Y1 N1 Si4B -171.5(3) . . . . ? O2 Y1 N1 Si3 -173.91(9) . . . . ? O1 Y1 N1 Si3 -2.98(15) . . . . ? O3 Y1 N1 Si3 91.77(11) . . . . ? N999 Y1 N1 Si3 -89.84(12) . . . . ? C2 Y1 N1 Si3 -18.62(13) . . . . ? Si4B Y1 N1 Si3 171.5(3) . . . . ? O2 Y1 N1 Si4A -7.78(17) . . . . ? O1 Y1 N1 Si4A 163.15(12) . . . . ? O3 Y1 N1 Si4A -102.10(14) . . . . ? N999 Y1 N1 Si4A 76.29(15) . . . . ? C2 Y1 N1 Si4A 147.51(14) . . . . ? Si3 Y1 N1 Si4A 166.1(2) . . . . ? Si4B Y1 N1 Si4A -22.37(16) . . . . ? Si4B N1 Si4A C4A 155.8(7) . . . . ? Si3 N1 Si4A C4A 77.6(3) . . . . ? Y1 N1 Si4A C4A -85.4(3) . . . . ? Si4B N1 Si4A C5A 33.5(5) . . . . ? Si3 N1 Si4A C5A -44.6(3) . . . . ? Y1 N1 Si4A C5A 152.4(3) . . . . ? Si3 N1 Si4B C4B 70.9(5) . . . . ? Si4A N1 Si4B C4B -45.8(6) . . . . ? Y1 N1 Si4B C4B -118.6(5) . . . . ? Si3 N1 Si4B C5B -57.6(5) . . . . ? Si4A N1 Si4B C5B -174.3(8) . . . . ? Y1 N1 Si4B C5B 113.0(5) . . . . ? Si3 N1 Si4B Y1 -170.6(3) . . . . ? Si4A N1 Si4B Y1 72.8(5) . . . . ? O2 Y1 Si4B N1 -167.03(18) . . . . ? O1 Y1 Si4B N1 8.2(2) . . . . ? O3 Y1 Si4B N1 104.19(19) . . . . ? N999 Y1 Si4B N1 -87.32(19) . . . . ? C2 Y1 Si4B N1 -12.3(2) . . . . ? Si3 Y1 Si4B N1 5.28(17) . . . . ? O2 Y1 Si4B C4B -87.9(4) . . . . ? O1 Y1 Si4B C4B 87.4(4) . . . . ? N1 Y1 Si4B C4B 79.2(5) . . . . ? O3 Y1 Si4B C4B -176.6(4) . . . . ? N999 Y1 Si4B C4B -8.1(4) . . . . ? C2 Y1 Si4B C4B 66.9(4) . . . . ? Si3 Y1 Si4B C4B 84.5(4) . . . . ? O2 Y1 Si4B C5B 106.5(4) . . . . ? O1 Y1 Si4B C5B -78.2(4) . . . . ? N1 Y1 Si4B C5B -86.4(4) . . . . ? O3 Y1 Si4B C5B 17.8(4) . . . . ? N999 Y1 Si4B C5B -173.8(4) . . . . ? C2 Y1 Si4B C5B -98.7(4) . . . . ? Si3 Y1 Si4B C5B -81.2(4) . . . . ? Si4B N1 Si3 C3A -81.7(2) . . . . ? Si4A N1 Si3 C3A -57.1(2) . . . . ? Y1 N1 Si3 C3A 106.61(14) . . . . ? Si4B N1 Si3 C3B 46.8(2) . . . . ? Si4A N1 Si3 C3B 71.4(2) . . . . ? Y1 N1 Si3 C3B -124.86(15) . . . . ? Si4B N1 Si3 Y1 171.7(3) . . . . ? Si4A N1 Si3 Y1 -163.7(3) . . . . ? O2 Y1 Si3 N1 9.83(14) . . . . ? O1 Y1 Si3 N1 177.51(13) . . . . ? O3 Y1 Si3 N1 -94.60(13) . . . . ? N999 Y1 Si3 N1 96.87(13) . . . . ? C2 Y1 Si3 N1 161.49(13) . . . . ? Si4B Y1 Si3 N1 -4.14(13) . . . . ? O2 Y1 Si3 C3A -83.79(14) . . . . ? O1 Y1 Si3 C3A 83.89(12) . . . . ? N1 Y1 Si3 C3A -93.61(17) . . . . ? O3 Y1 Si3 C3A 171.79(12) . . . . ? N999 Y1 Si3 C3A 3.26(12) . . . . ? C2 Y1 Si3 C3A 67.88(12) . . . . ? Si4B Y1 Si3 C3A -97.76(13) . . . . ? O2 Y1 Si3 C3B 90.58(18) . . . . ? O1 Y1 Si3 C3B -101.74(17) . . . . ? N1 Y1 Si3 C3B 80.8(2) . . . . ? O3 Y1 Si3 C3B -13.84(17) . . . . ? N999 Y1 Si3 C3B 177.63(17) . . . . ? C2 Y1 Si3 C3B -117.75(17) . . . . ? Si4B Y1 Si3 C3B 76.61(17) . . . . ? O1 Y1 O2 C22 -126.92(15) . . . . ? N1 Y1 O2 C22 44.44(17) . . . . ? O3 Y1 O2 C22 147.39(15) . . . . ? N999 Y1 O2 C22 -55.06(15) . . . . ? C2 Y1 O2 C22 -102.81(16) . . . . ? Si3 Y1 O2 C22 39.04(19) . . . . ? Si4B Y1 O2 C22 50.01(16) . . . . ? O2 Y1 O1 C2 129.87(14) . . . . ? N1 Y1 O1 C2 -40.97(17) . . . . ? O3 Y1 O1 C2 -143.90(14) . . . . ? N999 Y1 O1 C2 58.80(14) . . . . ? Si3 Y1 O1 C2 -42.42(14) . . . . ? Si4B Y1 O1 C2 -44.72(19) . . . . ? O2 Y1 O3 C31 61.30(15) . . . . ? O1 Y1 O3 C31 -57.51(15) . . . . ? N1 Y1 O3 C31 179.06(15) . . . . ? N999 Y1 O3 C31 2.6(2) . . . . ? C2 Y1 O3 C31 -71.64(15) . . . . ? Si3 Y1 O3 C31 -151.00(14) . . . . ? Si4B Y1 O3 C31 156.65(15) . . . . ? O2 Y1 O3 C34 -116.68(18) . . . . ? O1 Y1 O3 C34 124.50(18) . . . . ? N1 Y1 O3 C34 1.07(19) . . . . ? N999 Y1 O3 C34 -175.36(17) . . . . ? C2 Y1 O3 C34 110.38(18) . . . . ? Si3 Y1 O3 C34 31.02(18) . . . . ? Si4B Y1 O3 C34 -21.34(18) . . . . ? C34 O3 C31 C32 10.2(3) . . . . ? Y1 O3 C31 C32 -168.2(2) . . . . ? O3 C31 C32 C33 -21.1(4) . . . . ? C31 C32 C33 C34 24.2(4) . . . . ? C31 O3 C34 C33 4.2(3) . . . . ? Y1 O3 C34 C33 -177.73(19) . . . . ? C32 C33 C34 O3 -17.5(4) . . . . ? O2 Y1 N999 C11 -138.85(16) . . . . ? O1 Y1 N999 C11 -16.71(15) . . . . ? N1 Y1 N999 C11 105.30(17) . . . . ? O3 Y1 N999 C11 -78.3(2) . . . . ? C2 Y1 N999 C11 4.72(15) . . . . ? Si3 Y1 N999 C11 75.33(15) . . . . ? Si4B Y1 N999 C11 128.55(15) . . . . ? O2 Y1 N999 C15 13.20(16) . . . . ? O1 Y1 N999 C15 135.33(16) . . . . ? N1 Y1 N999 C15 -102.66(17) . . . . ? O3 Y1 N999 C15 73.8(2) . . . . ? C2 Y1 N999 C15 156.76(17) . . . . ? Si3 Y1 N999 C15 -132.63(15) . . . . ? Si4B Y1 N999 C15 -79.41(17) . . . . ? C11 N999 C15 C14 3.5(3) . . . . ? Y1 N999 C15 C14 -147.62(17) . . . . ? C11 N999 C15 C21 -177.6(2) . . . . ? Y1 N999 C15 C21 31.3(3) . . . . ? N999 C15 C21 C22 -56.5(3) . . . . ? C14 C15 C21 C22 122.5(2) . . . . ? N999 C15 C21 C29 129.8(2) . . . . ? C14 C15 C21 C29 -51.2(3) . . . . ? C22 C21 C29 C30 -4.4(3) . . . . ? C15 C21 C29 C30 169.3(2) . . . . ? C22 C21 C29 C28 174.4(2) . . . . ? C15 C21 C29 C28 -11.9(3) . . . . ? C30 C29 C28 C27 -2.4(3) . . . . ? C21 C29 C28 C27 178.8(2) . . . . ? C29 C28 C27 C26 0.1(4) . . . . ? C28 C27 C26 C25 1.9(4) . . . . ? C27 C26 C25 C30 -1.5(4) . . . . ? C26 C25 C30 C24 -179.3(2) . . . . ? C26 C25 C30 C29 -1.0(3) . . . . ? C28 C29 C30 C25 2.9(3) . . . . ? C21 C29 C30 C25 -178.3(2) . . . . ? C28 C29 C30 C24 -178.8(2) . . . . ? C21 C29 C30 C24 0.1(3) . . . . ? C25 C30 C24 C23 -179.4(2) . . . . ? C29 C30 C24 C23 2.3(3) . . . . ? C30 C24 C23 C22 -0.4(3) . . . . ? C30 C24 C23 Si2 -176.43(18) . . . . ? Y1 O2 C22 C21 52.8(3) . . . . ? Y1 O2 C22 C23 -128.35(17) . . . . ? C29 C21 C22 O2 -174.7(2) . . . . ? C15 C21 C22 O2 11.6(3) . . . . ? C29 C21 C22 C23 6.4(3) . . . . ? C15 C21 C22 C23 -167.2(2) . . . . ? C24 C23 C22 O2 177.1(2) . . . . ? Si2 C23 C22 O2 -7.0(3) . . . . ? C24 C23 C22 C21 -4.0(3) . . . . ? Si2 C23 C22 C21 171.87(17) . . . . ? C24 C23 Si2 C51 -137.5(2) . . . . ? C22 C23 Si2 C51 46.7(2) . . . . ? C24 C23 Si2 C52 -19.1(2) . . . . ? C22 C23 Si2 C52 165.00(19) . . . . ? C24 C23 Si2 C53 99.4(2) . . . . ? C22 C23 Si2 C53 -76.5(2) . . . . ? C51 Si2 C53 C56 -68.9(2) . . . . ? C52 Si2 C53 C56 172.8(2) . . . . ? C23 Si2 C53 C56 54.5(2) . . . . ? C51 Si2 C53 C55 172.13(19) . . . . ? C52 Si2 C53 C55 53.9(2) . . . . ? C23 Si2 C53 C55 -64.5(2) . . . . ? C51 Si2 C53 C54 52.3(2) . . . . ? C52 Si2 C53 C54 -65.9(2) . . . . ? C23 Si2 C53 C54 175.7(2) . . . . ? N999 C15 C14 C13 -1.6(3) . . . . ? C21 C15 C14 C13 179.4(2) . . . . ? C15 C14 C13 C12 -1.4(4) . . . . ? C15 N999 C11 C12 -2.4(3) . . . . ? Y1 N999 C11 C12 149.44(18) . . . . ? C15 N999 C11 C1 177.3(2) . . . . ? Y1 N999 C11 C1 -30.9(2) . . . . ? N999 C11 C1 C2 60.3(3) . . . . ? C12 C11 C1 C2 -120.1(2) . . . . ? N999 C11 C1 C9 -123.9(2) . . . . ? C12 C11 C1 C9 55.7(3) . . . . ? C2 C1 C9 C8 -172.3(2) . . . . ? C11 C1 C9 C8 11.9(3) . . . . ? C2 C1 C9 C10 4.2(3) . . . . ? C11 C1 C9 C10 -171.57(19) . . . . ? C10 C9 C8 C7 0.8(3) . . . . ? C1 C9 C8 C7 177.4(2) . . . . ? C9 C8 C7 C6 0.4(4) . . . . ? C8 C7 C6 C5 -1.0(4) . . . . ? C7 C6 C5 C10 0.3(4) . . . . ? C6 C5 C10 C4 -178.7(2) . . . . ? C6 C5 C10 C9 1.0(3) . . . . ? C8 C9 C10 C5 -1.5(3) . . . . ? C1 C9 C10 C5 -178.3(2) . . . . ? C8 C9 C10 C4 178.2(2) . . . . ? C1 C9 C10 C4 1.4(3) . . . . ? C5 C10 C4 C3 175.2(2) . . . . ? C9 C10 C4 C3 -4.5(3) . . . . ? C10 C4 C3 C2 1.8(3) . . . . ? C10 C4 C3 Si1 -178.15(18) . . . . ? Y1 O1 C2 C1 -55.2(2) . . . . ? Y1 O1 C2 C3 124.31(18) . . . . ? C9 C1 C2 O1 172.49(19) . . . . ? C11 C1 C2 O1 -11.8(3) . . . . ? C9 C1 C2 C3 -7.0(3) . . . . ? C11 C1 C2 C3 168.7(2) . . . . ? C9 C1 C2 Y1 140.30(18) . . . . ? C11 C1 C2 Y1 -44.0(2) . . . . ? C4 C3 C2 O1 -175.5(2) . . . . ? Si1 C3 C2 O1 4.5(3) . . . . ? C4 C3 C2 C1 4.0(3) . . . . ? Si1 C3 C2 C1 -176.01(17) . . . . ? C4 C3 C2 Y1 -128.0(2) . . . . ? Si1 C3 C2 Y1 52.0(3) . . . . ? O2 Y1 C2 O1 -64.23(16) . . . . ? N1 Y1 C2 O1 145.49(15) . . . . ? O3 Y1 C2 O1 37.75(15) . . . . ? N999 Y1 C2 O1 -115.35(15) . . . . ? Si3 Y1 C2 O1 136.26(14) . . . . ? Si4B Y1 C2 O1 150.32(13) . . . . ? O2 Y1 C2 C1 70.64(16) . . . . ? O1 Y1 C2 C1 134.9(2) . . . . ? N1 Y1 C2 C1 -79.64(15) . . . . ? O3 Y1 C2 C1 172.61(13) . . . . ? N999 Y1 C2 C1 19.52(13) . . . . ? Si3 Y1 C2 C1 -88.88(13) . . . . ? Si4B Y1 C2 C1 -74.81(15) . . . . ? O2 Y1 C2 C3 -149.3(2) . . . . ? O1 Y1 C2 C3 -85.1(2) . . . . ? N1 Y1 C2 C3 60.4(2) . . . . ? O3 Y1 C2 C3 -47.4(2) . . . . ? N999 Y1 C2 C3 159.6(2) . . . . ? Si3 Y1 C2 C3 51.2(2) . . . . ? Si4B Y1 C2 C3 65.2(2) . . . . ? C4 C3 Si1 C42 132.21(19) . . . . ? C2 C3 Si1 C42 -47.8(2) . . . . ? C4 C3 Si1 C41 15.8(2) . . . . ? C2 C3 Si1 C41 -164.16(19) . . . . ? C4 C3 Si1 C43 -102.8(2) . . . . ? C2 C3 Si1 C43 77.2(2) . . . . ? C42 Si1 C43 C44B 44.3(3) . . . . ? C41 Si1 C43 C44B 160.4(3) . . . . ? C3 Si1 C43 C44B -81.6(3) . . . . ? C42 Si1 C43 C45B 168.5(3) . . . . ? C41 Si1 C43 C45B -75.5(3) . . . . ? C3 Si1 C43 C45B 42.5(3) . . . . ? C42 Si1 C43 C46A -41.3(3) . . . . ? C41 Si1 C43 C46A 74.7(3) . . . . ? C3 Si1 C43 C46A -167.2(3) . . . . ? C42 Si1 C43 C46B -73.8(3) . . . . ? C41 Si1 C43 C46B 42.2(3) . . . . ? C3 Si1 C43 C46B 160.2(3) . . . . ? C42 Si1 C43 C45A -163.9(3) . . . . ? C41 Si1 C43 C45A -47.9(3) . . . . ? C3 Si1 C43 C45A 70.1(3) . . . . ? C42 Si1 C43 C44A 80.2(3) . . . . ? C41 Si1 C43 C44A -163.8(3) . . . . ? C3 Si1 C43 C44A -45.8(3) . . . . ? C14 C13 C12 C11 2.5(4) . . . . ? N999 C11 C12 C13 -0.6(3) . . . . ? C1 C11 C12 C13 179.7(2) . . . . ? C106 C101 C102 C103 0.2(5) . . . . ? C101 C102 C103 C104 -0.2(4) . . . . ? C102 C103 C104 C105 -0.1(4) . . . . ? C103 C104 C105 C106 0.6(4) . . . . ? C104 C105 C106 C101 -0.6(4) . . . . ? C102 C101 C106 C105 0.2(5) . . . . ? C116 C111 C112 C113 -0.2(4) . . . . ? C111 C112 C113 C114 -0.2(4) . . . . ? C112 C113 C114 C115 0.3(4) . . . . ? C113 C114 C115 C116 -0.1(4) . . . . ? C112 C111 C116 C115 0.5(4) . . . . ? C114 C115 C116 C111 -0.3(4) . . . . ? C123 C121 C122 C123 -0.2(6) 3_556 . . . ? C121 C122 C123 C121 0.2(6) . . . 3_556 ? #===END data_complex7 _database_code_depnum_ccdc_archive 'CCDC 752790' #TrackingRef 'Cif_files_B920283H.cif' _audit_creation_date 2009-02-05T19:13:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C68 H64 N O3 S Sc Si4, 4(C6 H6)' _chemical_formula_sum 'C92 H88 N O3 S Sc Si4' _chemical_formula_weight 1445.01 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3960(7) _cell_length_b 15.9382(10) _cell_length_c 21.8083(14) _cell_angle_alpha 103.867(4) _cell_angle_beta 98.581(4) _cell_angle_gamma 106.022(3) _cell_volume 3912.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3092 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 22.48 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.233 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.954 _exptl_absorpt_correction_T_max 0.986 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.1075 _diffrn_reflns_av_unetI/netI 0.1765 _diffrn_reflns_number 43820 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 17816 _reflns_number_gt 10227 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART, 2006' _computing_cell_refinement 'Bruker SMART, 2006' _computing_data_reduction 'Bruker SAINT, 2006' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0414P)^2^+6.8111P] 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_number_reflns 17816 _refine_ls_number_parameters 917 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1761 _refine_ls_R_factor_gt 0.1013 _refine_ls_wR_factor_ref 0.1954 _refine_ls_wR_factor_gt 0.1652 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.543 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.092 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 S1 S 0.74872(10) 0.22251(8) 0.89903(6) 0.0151(3) Uani 1 1 d . . . Sc1 Sc 0.91390(8) 0.17309(6) 0.83928(4) 0.0131(2) Uani 1 1 d . . . Si1 Si 1.23446(11) 0.37543(9) 1.02183(7) 0.0152(3) Uani 1 1 d . . . Si2 Si 0.73600(12) 0.18361(9) 0.62797(7) 0.0159(3) Uani 1 1 d . . . Si3 Si 0.93919(12) -0.00271(9) 0.89116(7) 0.0173(3) Uani 1 1 d . . . H3SI H 0.956(5) 0.064(4) 0.954(3) 0.05 Uiso 1 1 d . . . C3A C 1.0767(4) -0.0298(3) 0.8933(3) 0.023 Uani 1 1 d . . . H3A1 H 1.0638 -0.0863 0.8589 0.034 Uiso 1 1 calc R . . H3A2 H 1.1031 -0.0376 0.9356 0.034 Uiso 1 1 calc R . . H3A3 H 1.1355 0.0204 0.8864 0.034 Uiso 1 1 calc R . . C3B C 0.8244(5) -0.1092(3) 0.8883(3) 0.0264(13) Uani 1 1 d . . . H3B1 H 0.7525 -0.096 0.8917 0.04 Uiso 1 1 calc R . . H3B2 H 0.8486 -0.1314 0.9245 0.04 Uiso 1 1 calc R . . H3B3 H 0.8119 -0.1561 0.8472 0.04 Uiso 1 1 calc R . . Si4 Si 0.86308(12) -0.02477(9) 0.74809(7) 0.0167(3) Uani 1 1 d . . . H4SI H 0.905(5) 0.043(4) 0.711(3) 0.05 Uiso 1 1 d . . . C4A C 0.7042(4) -0.0793(3) 0.7203(2) 0.024 Uani 1 1 d . . . H4A1 H 0.6781 -0.1239 0.7435 0.036 Uiso 1 1 calc R . . H4A2 H 0.6839 -0.1103 0.6736 0.036 Uiso 1 1 calc R . . H4A3 H 0.6668 -0.0324 0.7292 0.036 Uiso 1 1 calc R . . C4B C 0.9266(4) -0.1191(3) 0.7278(2) 0.0244(12) Uani 1 1 d . . . H4B1 H 1.0109 -0.0931 0.7378 0.037 Uiso 1 1 calc R . . H4B2 H 0.8981 -0.1525 0.6814 0.037 Uiso 1 1 calc R . . H4B3 H 0.9041 -0.161 0.7534 0.037 Uiso 1 1 calc R . . O2 O 0.7900(3) 0.1685(2) 0.76659(16) 0.0163(7) Uani 1 1 d . . . N2 N 0.9056(3) 0.0414(3) 0.82868(19) 0.0170(9) Uani 1 1 d . . . O3 O 1.0581(3) 0.2198(2) 0.80000(16) 0.0193(8) Uani 1 1 d . . . O1 O 1.0007(3) 0.2433(2) 0.93038(16) 0.0170(7) Uani 1 1 d . . . C1 C 0.8894(4) 0.2239(3) 1.0103(2) 0.0140(10) Uani 1 1 d . . . C2 C 0.9940(4) 0.2604(3) 0.9927(2) 0.0146(10) Uani 1 1 d . . . C3 C 1.0967(4) 0.3153(3) 1.0419(2) 0.0146(10) Uani 1 1 d . . . C4 C 1.0927(4) 0.3246(3) 1.1063(2) 0.0155(10) Uani 1 1 d . . . H4 H 1.1608 0.3598 1.139 0.019 Uiso 1 1 calc R . . C5 C 0.9913(4) 0.2918(3) 1.1918(2) 0.0207(11) Uani 1 1 d . . . H5 H 1.0604 0.3245 1.2242 0.025 Uiso 1 1 calc R . . C6 C 0.8916(4) 0.2526(3) 1.2092(3) 0.0226(12) Uani 1 1 d . . . H6 H 0.8927 0.2558 1.2533 0.027 Uiso 1 1 calc R . . C7 C 0.7876(4) 0.2077(3) 1.1615(2) 0.0200(11) Uani 1 1 d . . . H7 H 0.7183 0.1829 1.1741 0.024 Uiso 1 1 calc R . . C8 C 0.7854(4) 0.1996(3) 1.0973(2) 0.0179(11) Uani 1 1 d . . . H8 H 0.7146 0.1691 1.0659 0.021 Uiso 1 1 calc R . . C9 C 0.8870(4) 0.2358(3) 1.0770(2) 0.0159(10) Uani 1 1 d . . . C10 C 0.9912(4) 0.2837(3) 1.1255(2) 0.0154(10) Uani 1 1 d . . . C11 C 0.7870(4) 0.1718(3) 0.9578(2) 0.0152(10) Uani 1 1 d . . . C12 C 0.7159(4) 0.0841(3) 0.9408(2) 0.0152(10) Uani 1 1 d . . . H12 H 0.7183 0.0456 0.9677 0.018 Uiso 1 1 calc R . . C31 C 1.1487(4) 0.1774(4) 0.7977(3) 0.0341(15) Uani 1 1 d . . . H31A H 1.1243 0.122 0.76 0.041 Uiso 1 1 calc R . . H31B H 1.1663 0.1601 0.8378 0.041 Uiso 1 1 calc R . . C32 C 1.2531(5) 0.2488(4) 0.7917(3) 0.0299(13) Uani 1 1 d . . . H32A H 1.3008 0.2202 0.7668 0.036 Uiso 1 1 calc R . . H32B H 1.3013 0.2882 0.8349 0.036 Uiso 1 1 calc R . . C33 C 1.1984(5) 0.3027(4) 0.7552(3) 0.0314(14) Uani 1 1 d . . . H33A H 1.252 0.3652 0.7636 0.038 Uiso 1 1 calc R . . H33B H 1.1764 0.2718 0.7079 0.038 Uiso 1 1 calc R . . C34 C 1.0929(4) 0.3050(3) 0.7818(3) 0.0247(12) Uani 1 1 d . . . H34A H 1.1119 0.3591 0.8201 0.03 Uiso 1 1 calc R . . H34B H 1.0307 0.3067 0.7484 0.03 Uiso 1 1 calc R . . C13 C 0.6367(4) 0.0545(3) 0.8787(2) 0.0171(11) Uani 1 1 d . . . H13 H 0.5829 -0.0055 0.8605 0.021 Uiso 1 1 calc R . . C14 C 0.6464(4) 0.1207(3) 0.8485(2) 0.0139(10) Uani 1 1 d . . . C21 C 0.5975(4) 0.1177(3) 0.7813(2) 0.0151(10) Uani 1 1 d . . . C22 C 0.6757(4) 0.1457(3) 0.7442(2) 0.0159(10) Uani 1 1 d . . . C23 C 0.6330(4) 0.1463(3) 0.6791(2) 0.0147(10) Uani 1 1 d . . . C24 C 0.5165(4) 0.1161(3) 0.6541(2) 0.0177(11) Uani 1 1 d . . . H24 H 0.4889 0.1179 0.6116 0.021 Uiso 1 1 calc R . . C25 C 0.3146(4) 0.0450(3) 0.6600(2) 0.0208(11) Uani 1 1 d . . . H25 H 0.2875 0.0443 0.6167 0.025 Uiso 1 1 calc R . . C26 C 0.2372(4) 0.0103(3) 0.6942(3) 0.0238(12) Uani 1 1 d . . . H26 H 0.1571 -0.015 0.6745 0.029 Uiso 1 1 calc R . . C27 C 0.2784(4) 0.0126(3) 0.7592(2) 0.0208(11) Uani 1 1 d . . . H27 H 0.2252 -0.0115 0.7828 0.025 Uiso 1 1 calc R . . C28 C 0.3923(4) 0.0487(3) 0.7881(3) 0.0195(11) Uani 1 1 d . . . H28 H 0.4172 0.0506 0.8319 0.023 Uiso 1 1 calc R . . C29 C 0.4755(4) 0.0838(3) 0.7545(2) 0.0155(10) Uani 1 1 d . . . C30 C 0.4342(4) 0.0818(3) 0.6892(2) 0.0150(10) Uani 1 1 d . . . C41 C 1.3275(4) 0.4682(3) 1.0975(2) 0.0141(10) Uani 1 1 d . . . C42 C 1.3344(5) 0.5596(3) 1.1068(3) 0.0270(13) Uani 1 1 d . . . H42 H 1.2908 0.5757 1.0745 0.032 Uiso 1 1 calc R . . C43 C 1.4047(5) 0.6278(3) 1.1628(3) 0.0298(13) Uani 1 1 d . . . H43 H 1.4078 0.6895 1.1684 0.036 Uiso 1 1 calc R . . C44 C 1.4695(5) 0.6059(4) 1.2101(3) 0.0271(13) Uani 1 1 d . . . H44 H 1.5175 0.6524 1.248 0.032 Uiso 1 1 calc R . . C45 C 1.4644(5) 0.5164(4) 1.2019(3) 0.0292(13) Uani 1 1 d . . . H45 H 1.5088 0.501 1.2342 0.035 Uiso 1 1 calc R . . C47 C 1.3242(4) 0.2997(3) 0.9986(2) 0.0183(11) Uani 1 1 d . . . C48 C 1.4405(4) 0.3386(3) 1.0022(3) 0.0232(12) Uani 1 1 d . . . H48 H 1.4729 0.4033 1.0141 0.028 Uiso 1 1 calc R . . C49 C 1.5117(4) 0.2850(4) 0.9889(3) 0.0251(12) Uani 1 1 d . . . H49 H 1.5911 0.3131 0.9912 0.03 Uiso 1 1 calc R . . C50 C 1.4657(5) 0.1917(4) 0.9724(3) 0.0311(14) Uani 1 1 d . . . H50 H 1.5136 0.1548 0.9644 0.037 Uiso 1 1 calc R . . C51 C 1.3496(5) 0.1515(4) 0.9677(3) 0.0304(14) Uani 1 1 d . . . H51 H 1.3178 0.0868 0.9558 0.036 Uiso 1 1 calc R . . C52 C 1.2787(4) 0.2047(3) 0.9801(3) 0.0235(12) Uani 1 1 d . . . H52 H 1.1987 0.1761 0.9759 0.028 Uiso 1 1 calc R . . C53 C 1.3944(4) 0.4487(4) 1.1466(3) 0.0259(12) Uani 1 1 d . . . H53 H 1.3916 0.3872 1.1417 0.031 Uiso 1 1 calc R . . C54 C 1.2090(4) 0.4374(3) 0.9608(2) 0.0170(10) Uani 1 1 d . . . C55 C 1.2927(4) 0.4659(3) 0.9268(2) 0.0200(11) Uani 1 1 d . . . H55 H 1.357 0.4444 0.9289 0.024 Uiso 1 1 calc R . . C56 C 1.2836(5) 0.5247(3) 0.8901(2) 0.0240(12) Uani 1 1 d . . . H56 H 1.3407 0.5425 0.8669 0.029 Uiso 1 1 calc R . . C57 C 1.1914(5) 0.5572(3) 0.8873(2) 0.0244(12) Uani 1 1 d . . . H57 H 1.1862 0.5985 0.8628 0.029 Uiso 1 1 calc R . . C58 C 1.1068(5) 0.5307(3) 0.9197(2) 0.0239(12) Uani 1 1 d . . . H58 H 1.043 0.5528 0.9172 0.029 Uiso 1 1 calc R . . C59 C 1.1160(4) 0.4709(3) 0.9561(2) 0.0218(11) Uani 1 1 d . . . H59 H 1.0575 0.4524 0.9783 0.026 Uiso 1 1 calc R . . C61 C 0.8379(4) 0.3025(3) 0.6687(2) 0.0158(10) Uani 1 1 d . . . C62 C 0.8288(4) 0.3570(3) 0.7285(3) 0.0224(12) Uani 1 1 d . . . H62 H 0.7701 0.3328 0.749 0.027 Uiso 1 1 calc R . . C63 C 0.9048(5) 0.4449(3) 0.7571(3) 0.0261(13) Uani 1 1 d . . . H63 H 0.8968 0.4811 0.7965 0.031 Uiso 1 1 calc R . . C64 C 0.9921(5) 0.4802(3) 0.7286(3) 0.0318(14) Uani 1 1 d . . . H64 H 1.0444 0.5404 0.7489 0.038 Uiso 1 1 calc R . . C65 C 1.0041(5) 0.4287(4) 0.6708(3) 0.0293(13) Uani 1 1 d . . . H65 H 1.0646 0.453 0.6514 0.035 Uiso 1 1 calc R . . C66 C 0.9269(4) 0.3413(3) 0.6414(3) 0.0227(12) Uani 1 1 d . . . H66 H 0.9348 0.3067 0.6013 0.027 Uiso 1 1 calc R . . C67 C 0.8122(4) 0.0983(3) 0.6044(2) 0.0171(10) Uani 1 1 d . . . C68 C 0.9301(4) 0.1199(3) 0.6081(2) 0.0222(12) Uani 1 1 d . . . H68 H 0.9778 0.182 0.6252 0.027 Uiso 1 1 calc R . . C69 C 0.9805(5) 0.0536(4) 0.5876(3) 0.0285(13) Uani 1 1 d . . . H69 H 1.0613 0.0701 0.5911 0.034 Uiso 1 1 calc R . . C70 C 0.9114(5) -0.0369(4) 0.5621(3) 0.0312(14) Uani 1 1 d . . . H70 H 0.9451 -0.0823 0.547 0.037 Uiso 1 1 calc R . . C71 C 0.7948(5) -0.0620(4) 0.5583(3) 0.0297(13) Uani 1 1 d . . . H71 H 0.7484 -0.1245 0.5418 0.036 Uiso 1 1 calc R . . C72 C 0.7450(5) 0.0058(3) 0.5792(2) 0.0236(12) Uani 1 1 d . . . H72 H 0.6642 -0.0113 0.5762 0.028 Uiso 1 1 calc R . . C73 C 0.6481(4) 0.1884(3) 0.5513(2) 0.0182(11) Uani 1 1 d . . . C74 C 0.6256(4) 0.1255(3) 0.4898(2) 0.0211(11) Uani 1 1 d . . . H74 H 0.6518 0.0741 0.4859 0.025 Uiso 1 1 calc R . . C75 C 0.5666(4) 0.1362(3) 0.4349(3) 0.0232(12) Uani 1 1 d . . . H75 H 0.5535 0.0929 0.3939 0.028 Uiso 1 1 calc R . . C76 C 0.5265(4) 0.2097(4) 0.4394(3) 0.0274(13) Uani 1 1 d . . . H76 H 0.4867 0.2172 0.4014 0.033 Uiso 1 1 calc R . . C77 C 0.5440(5) 0.2721(4) 0.4989(3) 0.0313(14) Uani 1 1 d . . . H77 H 0.5149 0.3219 0.5024 0.038 Uiso 1 1 calc R . . C78 C 0.6052(4) 0.2612(3) 0.5540(3) 0.0234(12) Uani 1 1 d . . . H78 H 0.6181 0.3049 0.5948 0.028 Uiso 1 1 calc R . . C101 C 0.4796(5) 0.7780(4) 0.7947(3) 0.0330(14) Uani 1 1 d . . . H101 H 0.5449 0.8214 0.8263 0.04 Uiso 1 1 calc R . . C102 C 0.4307(5) 0.8001(4) 0.7416(3) 0.0361(15) Uani 1 1 d . . . H102 H 0.4634 0.859 0.7371 0.043 Uiso 1 1 calc R . . C103 C 0.3367(5) 0.7389(4) 0.6959(3) 0.0366(15) Uani 1 1 d . . . H103 H 0.3035 0.7551 0.6602 0.044 Uiso 1 1 calc R . . C104 C 0.2904(5) 0.6523(4) 0.7024(3) 0.0360(15) Uani 1 1 d . . . H104 H 0.226 0.6085 0.6705 0.043 Uiso 1 1 calc R . . C105 C 0.3378(5) 0.6300(4) 0.7551(3) 0.0363(15) Uani 1 1 d . . . H105 H 0.3051 0.5711 0.7599 0.044 Uiso 1 1 calc R . . C106 C 0.4321(5) 0.6926(4) 0.8008(3) 0.0325(14) Uani 1 1 d . . . H106 H 0.4647 0.6768 0.8369 0.039 Uiso 1 1 calc R . . C111 C 0.0106(5) 0.6091(4) 0.5842(3) 0.0359(15) Uani 1 1 d . . . H111 H -0.0267 0.5541 0.593 0.043 Uiso 1 1 calc R . . C112 C -0.0155(5) 0.6876(4) 0.6090(3) 0.0330(14) Uani 1 1 d . . . H112 H -0.0705 0.6866 0.6351 0.04 Uiso 1 1 calc R . . C113 C 0.0385(5) 0.7679(4) 0.5957(3) 0.0339(14) Uani 1 1 d . . . H113 H 0.0205 0.8218 0.6128 0.041 Uiso 1 1 calc R . . C114 C 0.1188(5) 0.7694(4) 0.5575(3) 0.0371(15) Uani 1 1 d . . . H114 H 0.1554 0.8241 0.5482 0.045 Uiso 1 1 calc R . . C115 C 0.1457(5) 0.6906(4) 0.5329(3) 0.0319(14) Uani 1 1 d . . . H115 H 0.2008 0.6914 0.5069 0.038 Uiso 1 1 calc R . . C116 C 0.0916(5) 0.6111(4) 0.5464(3) 0.0345(14) Uani 1 1 d . . . H116 H 0.11 0.5573 0.5298 0.041 Uiso 1 1 calc R . . C121 C 0.6965(6) 0.5320(4) 0.5808(3) 0.0440(17) Uani 1 1 d . . . H121 H 0.7049 0.4978 0.5408 0.053 Uiso 1 1 calc R . . C122 C 0.7301(5) 0.5122(4) 0.6362(3) 0.0339(14) Uani 1 1 d . . . H122 H 0.7654 0.4662 0.6351 0.041 Uiso 1 1 calc R . . C123 C 0.7133(5) 0.5584(4) 0.6943(3) 0.0396(16) Uani 1 1 d . . . H123 H 0.7346 0.5426 0.7326 0.048 Uiso 1 1 calc R . . C124 C 0.6668(6) 0.6257(5) 0.6967(4) 0.061(2) Uani 1 1 d . . . H124 H 0.6574 0.6585 0.737 0.073 Uiso 1 1 calc R . . C125 C 0.6334(9) 0.6471(6) 0.6423(6) 0.096(3) Uani 1 1 d . . . H125 H 0.5981 0.6933 0.6441 0.115 Uiso 1 1 calc R . . C126 C 0.6508(7) 0.6007(6) 0.5823(5) 0.078(3) Uani 1 1 d . . . H126 H 0.631 0.6172 0.5441 0.093 Uiso 1 1 calc R . . C131 C 0.1934(6) 0.3685(6) 0.5602(3) 0.0526(19) Uani 1 1 d . . . H131 H 0.1284 0.3808 0.5401 0.063 Uiso 1 1 calc R . . C132 C 0.1863(7) 0.2846(5) 0.5617(3) 0.059(2) Uani 1 1 d . . . H132 H 0.1156 0.2361 0.5421 0.07 Uiso 1 1 calc R . . C135 C 0.3893(12) 0.4183(13) 0.6168(6) 0.170(11) Uani 1 1 d . . . H135 H 0.4612 0.4655 0.6358 0.204 Uiso 1 1 calc R . . C134 C 0.3771(12) 0.3350(16) 0.6171(6) 0.167(11) Uani 1 1 d . . . H134 H 0.4414 0.3218 0.637 0.201 Uiso 1 1 calc R . . C133 C 0.2776(13) 0.2672(8) 0.5904(5) 0.105(5) Uani 1 1 d . . . H133 H 0.2715 0.2069 0.5917 0.126 Uiso 1 1 calc R . . C136 C 0.2953(12) 0.4366(6) 0.5881(4) 0.093(4) Uani 1 1 d . . . H136 H 0.3018 0.4973 0.5878 0.112 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 S1 0.0158(6) 0.0163(6) 0.0136(7) 0.0047(5) 0.0030(5) 0.0060(5) Sc1 0.0131(5) 0.0159(4) 0.0113(5) 0.0039(4) 0.0026(4) 0.0063(4) Si1 0.0152(7) 0.0150(6) 0.0149(8) 0.0033(6) 0.0020(6) 0.0059(6) Si2 0.0172(7) 0.0174(7) 0.0132(8) 0.0053(6) 0.0033(6) 0.0052(6) Si3 0.0216(8) 0.0188(7) 0.0141(8) 0.0056(6) 0.0042(6) 0.0097(6) C3A 0.025 0.023 0.023 0.008 0.003 0.013 C3B 0.033(3) 0.028(3) 0.026(3) 0.014(3) 0.011(3) 0.015(3) Si4 0.0185(7) 0.0171(7) 0.0137(8) 0.0038(6) 0.0033(6) 0.0053(6) C4A 0.025 0.024 0.016 0 0.001 0.004 C4B 0.028(3) 0.030(3) 0.013(3) 0.001(2) 0.004(2) 0.013(2) O2 0.0121(17) 0.0210(17) 0.0166(19) 0.0068(15) 0.0031(14) 0.0056(14) N2 0.021(2) 0.023(2) 0.007(2) 0.0046(17) 0.0016(17) 0.0081(18) O3 0.0194(18) 0.0238(18) 0.018(2) 0.0068(15) 0.0055(15) 0.0113(15) O1 0.0200(18) 0.0202(17) 0.0122(19) 0.0061(14) 0.0041(15) 0.0074(15) C1 0.016(2) 0.014(2) 0.011(3) 0.0035(19) 0.000(2) 0.0045(19) C2 0.023(3) 0.015(2) 0.010(3) 0.0025(19) 0.006(2) 0.011(2) C3 0.014(2) 0.014(2) 0.017(3) 0.006(2) 0.004(2) 0.0047(19) C4 0.015(2) 0.015(2) 0.016(3) 0.004(2) 0.001(2) 0.005(2) C5 0.023(3) 0.023(3) 0.015(3) 0.004(2) 0.003(2) 0.007(2) C6 0.027(3) 0.024(3) 0.018(3) 0.004(2) 0.006(2) 0.011(2) C7 0.022(3) 0.021(3) 0.021(3) 0.010(2) 0.011(2) 0.008(2) C8 0.022(3) 0.017(2) 0.013(3) 0.001(2) 0.000(2) 0.010(2) C9 0.020(3) 0.014(2) 0.015(3) 0.003(2) 0.003(2) 0.009(2) C10 0.016(2) 0.014(2) 0.015(3) 0.002(2) 0.002(2) 0.006(2) C11 0.013(2) 0.020(2) 0.015(3) 0.008(2) 0.004(2) 0.007(2) C12 0.015(2) 0.021(2) 0.015(3) 0.009(2) 0.007(2) 0.009(2) C31 0.024(3) 0.032(3) 0.061(5) 0.024(3) 0.019(3) 0.019(3) C32 0.024(3) 0.028(3) 0.041(4) 0.010(3) 0.013(3) 0.009(2) C33 0.033(3) 0.031(3) 0.034(4) 0.020(3) 0.014(3) 0.004(3) C34 0.021(3) 0.020(3) 0.032(3) 0.013(2) 0.001(2) 0.004(2) C13 0.017(3) 0.016(2) 0.016(3) 0.002(2) 0.002(2) 0.004(2) C14 0.010(2) 0.019(2) 0.012(3) 0.005(2) 0.004(2) 0.0026(19) C21 0.012(2) 0.016(2) 0.014(3) 0.002(2) -0.003(2) 0.0033(19) C22 0.021(3) 0.014(2) 0.014(3) 0.001(2) 0.004(2) 0.011(2) C23 0.017(3) 0.017(2) 0.011(3) 0.005(2) 0.003(2) 0.006(2) C24 0.023(3) 0.018(2) 0.011(3) 0.001(2) -0.001(2) 0.009(2) C25 0.021(3) 0.025(3) 0.013(3) 0.003(2) 0.001(2) 0.006(2) C26 0.017(3) 0.025(3) 0.027(3) 0.006(2) 0.003(2) 0.006(2) C27 0.016(3) 0.026(3) 0.020(3) 0.007(2) 0.006(2) 0.007(2) C28 0.018(3) 0.019(2) 0.020(3) 0.007(2) 0.003(2) 0.005(2) C29 0.014(2) 0.016(2) 0.013(3) -0.002(2) 0.003(2) 0.005(2) C30 0.014(2) 0.014(2) 0.016(3) 0.004(2) 0.002(2) 0.0054(19) C41 0.013(2) 0.016(2) 0.017(3) 0.007(2) 0.007(2) 0.007(2) C42 0.032(3) 0.022(3) 0.026(3) 0.008(2) 0.000(3) 0.011(2) C43 0.039(3) 0.014(2) 0.028(3) 0.001(2) -0.002(3) 0.006(2) C44 0.025(3) 0.029(3) 0.017(3) -0.001(2) 0.001(2) 0.003(2) C45 0.031(3) 0.037(3) 0.020(3) 0.007(3) 0.003(3) 0.015(3) C47 0.016(3) 0.026(3) 0.011(3) 0.003(2) 0.000(2) 0.007(2) C48 0.018(3) 0.019(2) 0.030(3) 0.004(2) 0.005(2) 0.006(2) C49 0.009(2) 0.032(3) 0.028(3) 0.002(2) 0.003(2) 0.005(2) C50 0.026(3) 0.035(3) 0.036(4) 0.005(3) 0.009(3) 0.019(3) C51 0.030(3) 0.021(3) 0.038(4) 0.001(3) 0.005(3) 0.013(2) C52 0.018(3) 0.025(3) 0.026(3) 0.005(2) 0.004(2) 0.010(2) C53 0.026(3) 0.024(3) 0.028(3) 0.007(2) 0.001(2) 0.012(2) C54 0.017(3) 0.017(2) 0.013(3) 0.002(2) -0.002(2) 0.002(2) C55 0.024(3) 0.018(2) 0.016(3) 0.002(2) 0.002(2) 0.008(2) C56 0.026(3) 0.023(3) 0.017(3) 0.005(2) 0.005(2) -0.001(2) C57 0.034(3) 0.019(3) 0.015(3) 0.006(2) -0.002(2) 0.003(2) C58 0.034(3) 0.026(3) 0.017(3) 0.008(2) 0.006(2) 0.017(3) C59 0.027(3) 0.026(3) 0.016(3) 0.006(2) 0.008(2) 0.011(2) C61 0.024(3) 0.018(2) 0.009(3) 0.007(2) 0.003(2) 0.011(2) C62 0.027(3) 0.021(3) 0.021(3) 0.007(2) 0.003(2) 0.012(2) C63 0.037(3) 0.018(3) 0.022(3) 0.002(2) -0.001(3) 0.015(2) C64 0.035(3) 0.013(2) 0.039(4) 0.006(2) -0.004(3) 0.003(2) C65 0.026(3) 0.024(3) 0.037(4) 0.014(3) 0.004(3) 0.004(2) C66 0.024(3) 0.027(3) 0.019(3) 0.011(2) 0.004(2) 0.009(2) C67 0.022(3) 0.023(3) 0.004(2) 0.004(2) -0.001(2) 0.007(2) C68 0.027(3) 0.023(3) 0.019(3) 0.009(2) 0.006(2) 0.010(2) C69 0.029(3) 0.042(3) 0.031(3) 0.019(3) 0.020(3) 0.024(3) C70 0.053(4) 0.036(3) 0.022(3) 0.012(3) 0.018(3) 0.034(3) C71 0.043(4) 0.020(3) 0.023(3) 0.004(2) 0.009(3) 0.007(3) C72 0.028(3) 0.030(3) 0.017(3) 0.008(2) 0.006(2) 0.013(2) C73 0.015(2) 0.022(2) 0.019(3) 0.008(2) 0.008(2) 0.005(2) C74 0.027(3) 0.023(3) 0.015(3) 0.008(2) 0.004(2) 0.007(2) C75 0.026(3) 0.021(3) 0.017(3) 0.004(2) 0.000(2) 0.004(2) C76 0.023(3) 0.039(3) 0.019(3) 0.012(3) -0.001(2) 0.008(3) C77 0.038(3) 0.039(3) 0.024(3) 0.008(3) 0.003(3) 0.026(3) C78 0.024(3) 0.028(3) 0.017(3) 0.003(2) 0.003(2) 0.011(2) C101 0.018(3) 0.040(3) 0.038(4) 0.009(3) 0.009(3) 0.007(3) C102 0.036(4) 0.035(3) 0.046(4) 0.020(3) 0.024(3) 0.010(3) C103 0.039(4) 0.053(4) 0.021(3) 0.018(3) 0.013(3) 0.012(3) C104 0.036(4) 0.037(3) 0.028(4) 0.002(3) 0.007(3) 0.008(3) C105 0.033(3) 0.030(3) 0.048(4) 0.019(3) 0.010(3) 0.007(3) C106 0.030(3) 0.033(3) 0.044(4) 0.016(3) 0.011(3) 0.018(3) C111 0.036(4) 0.036(3) 0.035(4) 0.018(3) 0.005(3) 0.005(3) C112 0.030(3) 0.043(3) 0.018(3) 0.002(3) 0.004(3) 0.006(3) C113 0.032(3) 0.031(3) 0.033(4) 0.002(3) 0.008(3) 0.008(3) C114 0.033(3) 0.033(3) 0.038(4) 0.009(3) 0.008(3) 0.001(3) C115 0.030(3) 0.042(3) 0.022(3) 0.008(3) 0.007(3) 0.009(3) C116 0.037(4) 0.033(3) 0.032(4) 0.010(3) 0.001(3) 0.015(3) C121 0.049(4) 0.044(4) 0.047(5) 0.021(3) 0.009(3) 0.020(3) C122 0.026(3) 0.026(3) 0.052(4) 0.018(3) 0.008(3) 0.008(3) C123 0.031(3) 0.034(3) 0.045(4) 0.010(3) -0.004(3) 0.003(3) C124 0.062(5) 0.047(4) 0.059(6) -0.008(4) -0.002(4) 0.022(4) C125 0.111(8) 0.075(6) 0.130(10) 0.048(7) 0.014(7) 0.068(6) C126 0.077(6) 0.098(7) 0.087(8) 0.062(6) 0.018(5) 0.046(6) C131 0.047(5) 0.087(6) 0.031(4) 0.014(4) 0.012(3) 0.035(4) C132 0.076(6) 0.048(4) 0.029(4) -0.004(3) 0.022(4) -0.006(4) C135 0.068(9) 0.29(2) 0.018(6) -0.025(11) 0.008(6) -0.088(12) C134 0.085(10) 0.44(3) 0.034(7) 0.067(15) 0.034(8) 0.172(17) C133 0.212(14) 0.145(10) 0.047(7) 0.052(7) 0.072(8) 0.155(11) C136 0.161(11) 0.054(5) 0.041(6) 0.004(4) 0.046(7) -0.005(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S1 C11 1.746(5) . ? S1 C14 1.746(5) . ? S1 Sc1 2.7758(14) . ? Sc1 O1 1.997(3) . ? Sc1 O2 2.008(3) . ? Sc1 N2 2.027(4) . ? Sc1 O3 2.124(3) . ? Sc1 Si4 3.1337(16) . ? Si1 C54 1.877(5) . ? Si1 C3 1.884(5) . ? Si1 C41 1.887(5) . ? Si1 C47 1.889(5) . ? Si2 C61 1.874(5) . ? Si2 C67 1.877(5) . ? Si2 C73 1.884(5) . ? Si2 C23 1.885(5) . ? Si3 N2 1.725(4) . ? Si3 C3A 1.867(5) . ? Si3 C3B 1.871(5) . ? Si3 H3SI 1.48(6) . ? C3A H3A1 0.98 . ? C3A H3A2 0.98 . ? C3A H3A3 0.98 . ? C3B H3B1 0.98 . ? C3B H3B2 0.98 . ? C3B H3B3 0.98 . ? Si4 N2 1.734(4) . ? Si4 C4A 1.857(5) . ? Si4 C4B 1.875(5) . ? Si4 H4SI 1.53(6) . ? C4A H4A1 0.98 . ? C4A H4A2 0.98 . ? C4A H4A3 0.98 . ? C4B H4B1 0.98 . ? C4B H4B2 0.98 . ? C4B H4B3 0.98 . ? O2 C22 1.342(5) . ? O3 C31 1.463(5) . ? O3 C34 1.474(5) . ? O1 C2 1.341(5) . ? C1 C2 1.415(6) . ? C1 C9 1.429(6) . ? C1 C11 1.462(6) . ? C2 C3 1.436(7) . ? C3 C4 1.386(6) . ? C4 C10 1.422(6) . ? C4 H4 0.95 . ? C5 C6 1.374(7) . ? C5 C10 1.419(6) . ? C5 H5 0.95 . ? C6 C7 1.410(7) . ? C6 H6 0.95 . ? C7 C8 1.371(6) . ? C7 H7 0.95 . ? C8 C9 1.415(7) . ? C8 H8 0.95 . ? C9 C10 1.424(7) . ? C11 C12 1.357(6) . ? C12 C13 1.436(7) . ? C12 H12 0.95 . ? C31 C32 1.516(7) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.521(7) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 C34 1.513(7) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C13 C14 1.360(6) . ? C13 H13 0.95 . ? C14 C21 1.483(7) . ? C21 C22 1.401(6) . ? C21 C29 1.434(6) . ? C22 C23 1.441(7) . ? C23 C24 1.368(6) . ? C24 C30 1.431(6) . ? C24 H24 0.95 . ? C25 C26 1.379(7) . ? C25 C30 1.418(7) . ? C25 H25 0.95 . ? C26 C27 1.421(7) . ? C26 H26 0.95 . ? C27 C28 1.354(7) . ? C27 H27 0.95 . ? C28 C29 1.420(6) . ? C28 H28 0.95 . ? C29 C30 1.430(7) . ? C41 C42 1.398(6) . ? C41 C53 1.403(7) . ? C42 C43 1.398(7) . ? C42 H42 0.95 . ? C43 C44 1.381(8) . ? C43 H43 0.95 . ? C44 C45 1.378(7) . ? C44 H44 0.95 . ? C45 C53 1.385(7) . ? C45 H45 0.95 . ? C47 C48 1.385(7) . ? C47 C52 1.393(7) . ? C48 C49 1.402(6) . ? C48 H48 0.95 . ? C49 C50 1.372(7) . ? C49 H49 0.95 . ? C50 C51 1.381(7) . ? C50 H50 0.95 . ? C51 C52 1.392(7) . ? C51 H51 0.95 . ? C52 H52 0.95 . ? C53 H53 0.95 . ? C54 C59 1.397(6) . ? C54 C55 1.401(6) . ? C55 C56 1.386(7) . ? C55 H55 0.95 . ? C56 C57 1.379(7) . ? C56 H56 0.95 . ? C57 C58 1.376(7) . ? C57 H57 0.95 . ? C58 C59 1.397(7) . ? C58 H58 0.95 . ? C59 H59 0.95 . ? C61 C66 1.398(7) . ? C61 C62 1.420(6) . ? C62 C63 1.384(7) . ? C62 H62 0.95 . ? C63 C64 1.380(8) . ? C63 H63 0.95 . ? C64 C65 1.383(7) . ? C64 H64 0.95 . ? C65 C66 1.386(7) . ? C65 H65 0.95 . ? C66 H66 0.95 . ? C67 C68 1.392(7) . ? C67 C72 1.402(7) . ? C68 C69 1.387(7) . ? C68 H68 0.95 . ? C69 C70 1.384(8) . ? C69 H69 0.95 . ? C70 C71 1.372(8) . ? C70 H70 0.95 . ? C71 C72 1.405(7) . ? C71 H71 0.95 . ? C72 H72 0.95 . ? C73 C78 1.397(7) . ? C73 C74 1.404(7) . ? C74 C75 1.379(7) . ? C74 H74 0.95 . ? C75 C76 1.382(7) . ? C75 H75 0.95 . ? C76 C77 1.378(7) . ? C76 H76 0.95 . ? C77 C78 1.395(7) . ? C77 H77 0.95 . ? C78 H78 0.95 . ? C101 C106 1.373(7) . ? C101 C102 1.392(8) . ? C101 H101 0.95 . ? C102 C103 1.365(8) . ? C102 H102 0.95 . ? C103 C104 1.391(8) . ? C103 H103 0.95 . ? C104 C105 1.380(8) . ? C104 H104 0.95 . ? C105 C106 1.374(8) . ? C105 H105 0.95 . ? C106 H106 0.95 . ? C111 C112 1.383(8) . ? C111 C116 1.390(8) . ? C111 H111 0.95 . ? C112 C113 1.390(8) . ? C112 H112 0.95 . ? C113 C114 1.389(7) . ? C113 H113 0.95 . ? C114 C115 1.391(8) . ? C114 H114 0.95 . ? C115 C116 1.383(8) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C122 1.355(8) . ? C121 C126 1.361(9) . ? C121 H121 0.95 . ? C122 C123 1.381(8) . ? C122 H122 0.95 . ? C123 C124 1.345(9) . ? C123 H123 0.95 . ? C124 C125 1.350(11) . ? C124 H124 0.95 . ? C125 C126 1.418(12) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C132 1.324(10) . ? C131 C136 1.357(12) . ? C131 H131 0.95 . ? C132 C133 1.341(12) . ? C132 H132 0.95 . ? C135 C134 1.30(2) . ? C135 C136 1.374(19) . ? C135 H135 0.95 . ? C134 C133 1.333(19) . ? C134 H134 0.95 . ? C133 H133 0.95 . ? C136 H136 0.95 . ? 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 C11 S1 C14 93.2(2) . . ? C11 S1 Sc1 87.79(15) . . ? C14 S1 Sc1 88.42(15) . . ? O1 Sc1 O2 143.37(13) . . ? O1 Sc1 N2 106.27(15) . . ? O2 Sc1 N2 105.54(15) . . ? O1 Sc1 O3 93.18(13) . . ? O2 Sc1 O3 98.04(13) . . ? N2 Sc1 O3 101.18(14) . . ? O1 Sc1 S1 76.03(9) . . ? O2 Sc1 S1 74.91(9) . . ? N2 Sc1 S1 113.66(12) . . ? O3 Sc1 S1 145.12(10) . . ? O1 Sc1 Si4 135.78(10) . . ? O2 Sc1 Si4 79.33(10) . . ? N2 Sc1 Si4 30.72(11) . . ? O3 Sc1 Si4 89.39(9) . . ? S1 Sc1 Si4 121.58(5) . . ? C54 Si1 C3 112.2(2) . . ? C54 Si1 C41 104.7(2) . . ? C3 Si1 C41 107.9(2) . . ? C54 Si1 C47 112.3(2) . . ? C3 Si1 C47 113.7(2) . . ? C41 Si1 C47 105.2(2) . . ? C61 Si2 C67 112.8(2) . . ? C61 Si2 C73 106.0(2) . . ? C67 Si2 C73 107.9(2) . . ? C61 Si2 C23 111.5(2) . . ? C67 Si2 C23 110.9(2) . . ? C73 Si2 C23 107.5(2) . . ? N2 Si3 C3A 113.0(2) . . ? N2 Si3 C3B 113.2(2) . . ? C3A Si3 C3B 107.1(2) . . ? N2 Si3 H3SI 111(2) . . ? C3A Si3 H3SI 106(2) . . ? C3B Si3 H3SI 107(2) . . ? Si3 C3A H3A1 109.5 . . ? Si3 C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? Si3 C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? Si3 C3B H3B1 109.5 . . ? Si3 C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? Si3 C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? N2 Si4 C4A 112.5(2) . . ? N2 Si4 C4B 115.3(2) . . ? C4A Si4 C4B 106.3(2) . . ? C4A Si4 Sc1 108.08(16) . . ? C4B Si4 Sc1 142.98(18) . . ? N2 Si4 H4SI 104(2) . . ? C4A Si4 H4SI 110(2) . . ? C4B Si4 H4SI 109(2) . . ? Sc1 Si4 H4SI 72(2) . . ? Si4 C4A H4A1 109.5 . . ? Si4 C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? Si4 C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? Si4 C4B H4B1 109.5 . . ? Si4 C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? Si4 C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C22 O2 Sc1 144.8(3) . . ? Si3 N2 Si4 122.1(2) . . ? Si3 N2 Sc1 125.3(2) . . ? Si4 N2 Sc1 112.6(2) . . ? C31 O3 C34 109.8(4) . . ? C31 O3 Sc1 122.6(3) . . ? C34 O3 Sc1 126.8(3) . . ? C2 O1 Sc1 144.2(3) . . ? C2 C1 C9 120.2(4) . . ? C2 C1 C11 117.6(4) . . ? C9 C1 C11 122.2(4) . . ? O1 C2 C1 121.3(4) . . ? O1 C2 C3 118.3(4) . . ? C1 C2 C3 120.4(4) . . ? C4 C3 C2 118.2(4) . . ? C4 C3 Si1 119.4(4) . . ? C2 C3 Si1 122.4(4) . . ? C3 C4 C10 122.8(4) . . ? C3 C4 H4 118.6 . . ? C10 C4 H4 118.6 . . ? C6 C5 C10 120.2(5) . . ? C6 C5 H5 119.9 . . ? C10 C5 H5 119.9 . . ? C5 C6 C7 120.1(5) . . ? C5 C6 H6 120 . . ? C7 C6 H6 120 . . ? C8 C7 C6 120.6(5) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 121.1(5) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C8 C9 C10 118.1(4) . . ? C8 C9 C1 122.6(4) . . ? C10 C9 C1 119.3(4) . . ? C5 C10 C4 121.3(4) . . ? C5 C10 C9 119.9(4) . . ? C4 C10 C9 118.8(4) . . ? C12 C11 C1 132.2(4) . . ? C12 C11 S1 109.0(4) . . ? C1 C11 S1 118.4(3) . . ? C11 C12 C13 114.5(4) . . ? C11 C12 H12 122.8 . . ? C13 C12 H12 122.8 . . ? O3 C31 C32 105.8(4) . . ? O3 C31 H31A 110.6 . . ? C32 C31 H31A 110.6 . . ? O3 C31 H31B 110.6 . . ? C32 C31 H31B 110.6 . . ? H31A C31 H31B 108.7 . . ? C31 C32 C33 102.4(4) . . ? C31 C32 H32A 111.3 . . ? C33 C32 H32A 111.3 . . ? C31 C32 H32B 111.3 . . ? C33 C32 H32B 111.3 . . ? H32A C32 H32B 109.2 . . ? C34 C33 C32 104.2(4) . . ? C34 C33 H33A 110.9 . . ? C32 C33 H33A 110.9 . . ? C34 C33 H33B 110.9 . . ? C32 C33 H33B 110.9 . . ? H33A C33 H33B 108.9 . . ? O3 C34 C33 104.5(4) . . ? O3 C34 H34A 110.8 . . ? C33 C34 H34A 110.8 . . ? O3 C34 H34B 110.9 . . ? C33 C34 H34B 110.9 . . ? H34A C34 H34B 108.9 . . ? C14 C13 C12 113.3(4) . . ? C14 C13 H13 123.3 . . ? C12 C13 H13 123.3 . . ? C13 C14 C21 132.0(4) . . ? C13 C14 S1 109.6(4) . . ? C21 C14 S1 118.0(3) . . ? C22 C21 C29 121.3(4) . . ? C22 C21 C14 117.3(4) . . ? C29 C21 C14 121.4(4) . . ? O2 C22 C21 121.6(4) . . ? O2 C22 C23 118.7(4) . . ? C21 C22 C23 119.6(4) . . ? C24 C23 C22 119.0(4) . . ? C24 C23 Si2 120.3(4) . . ? C22 C23 Si2 120.6(4) . . ? C23 C24 C30 122.9(5) . . ? C23 C24 H24 118.6 . . ? C30 C24 H24 118.6 . . ? C26 C25 C30 120.2(5) . . ? C26 C25 H25 119.9 . . ? C30 C25 H25 119.9 . . ? C25 C26 C27 119.5(5) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C28 C27 C26 121.0(5) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 121.7(5) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? C28 C29 C30 117.4(4) . . ? C28 C29 C21 124.0(5) . . ? C30 C29 C21 118.5(4) . . ? C25 C30 C29 120.2(4) . . ? C25 C30 C24 121.3(5) . . ? C29 C30 C24 118.5(4) . . ? C42 C41 C53 117.0(5) . . ? C42 C41 Si1 121.6(4) . . ? C53 C41 Si1 121.4(4) . . ? C43 C42 C41 121.0(5) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C44 C43 C42 120.4(5) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C45 C44 C43 119.6(5) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C53 120.1(5) . . ? C44 C45 H45 119.9 . . ? C53 C45 H45 119.9 . . ? C48 C47 C52 117.9(4) . . ? C48 C47 Si1 119.8(4) . . ? C52 C47 Si1 122.3(4) . . ? C47 C48 C49 121.7(5) . . ? C47 C48 H48 119.2 . . ? C49 C48 H48 119.2 . . ? C50 C49 C48 119.5(5) . . ? C50 C49 H49 120.3 . . ? C48 C49 H49 120.3 . . ? C49 C50 C51 119.8(5) . . ? C49 C50 H50 120.1 . . ? C51 C50 H50 120.1 . . ? C50 C51 C52 120.7(5) . . ? C50 C51 H51 119.6 . . ? C52 C51 H51 119.6 . . ? C47 C52 C51 120.4(5) . . ? C47 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C45 C53 C41 121.9(5) . . ? C45 C53 H53 119.1 . . ? C41 C53 H53 119.1 . . ? C59 C54 C55 117.1(5) . . ? C59 C54 Si1 120.9(4) . . ? C55 C54 Si1 121.0(4) . . ? C56 C55 C54 121.4(5) . . ? C56 C55 H55 119.3 . . ? C54 C55 H55 119.3 . . ? C57 C56 C55 119.9(5) . . ? C57 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C58 C57 C56 120.7(5) . . ? C58 C57 H57 119.6 . . ? C56 C57 H57 119.6 . . ? C57 C58 C59 119.1(5) . . ? C57 C58 H58 120.4 . . ? C59 C58 H58 120.4 . . ? C58 C59 C54 121.8(5) . . ? C58 C59 H59 119.1 . . ? C54 C59 H59 119.1 . . ? C66 C61 C62 117.0(5) . . ? C66 C61 Si2 121.0(4) . . ? C62 C61 Si2 122.0(4) . . ? C63 C62 C61 120.6(5) . . ? C63 C62 H62 119.7 . . ? C61 C62 H62 119.7 . . ? C64 C63 C62 120.4(5) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 C65 120.5(5) . . ? C63 C64 H64 119.8 . . ? C65 C64 H64 119.8 . . ? C64 C65 C66 119.3(5) . . ? C64 C65 H65 120.4 . . ? C66 C65 H65 120.4 . . ? C65 C66 C61 122.2(5) . . ? C65 C66 H66 118.9 . . ? C61 C66 H66 118.9 . . ? C68 C67 C72 117.1(4) . . ? C68 C67 Si2 125.1(4) . . ? C72 C67 Si2 117.7(4) . . ? C69 C68 C67 122.1(5) . . ? C69 C68 H68 118.9 . . ? C67 C68 H68 118.9 . . ? C70 C69 C68 119.2(5) . . ? C70 C69 H69 120.4 . . ? C68 C69 H69 120.4 . . ? C71 C70 C69 121.0(5) . . ? C71 C70 H70 119.5 . . ? C69 C70 H70 119.5 . . ? C70 C71 C72 119.2(5) . . ? C70 C71 H71 120.4 . . ? C72 C71 H71 120.4 . . ? C67 C72 C71 121.3(5) . . ? C67 C72 H72 119.4 . . ? C71 C72 H72 119.4 . . ? C78 C73 C74 116.3(5) . . ? C78 C73 Si2 118.9(4) . . ? C74 C73 Si2 124.8(4) . . ? C75 C74 C73 121.8(5) . . ? C75 C74 H74 119.1 . . ? C73 C74 H74 119.1 . . ? C74 C75 C76 120.3(5) . . ? C74 C75 H75 119.9 . . ? C76 C75 H75 119.9 . . ? C77 C76 C75 120.2(5) . . ? C77 C76 H76 119.9 . . ? C75 C76 H76 119.9 . . ? C76 C77 C78 119.0(5) . . ? C76 C77 H77 120.5 . . ? C78 C77 H77 120.5 . . ? C77 C78 C73 122.5(5) . . ? C77 C78 H78 118.7 . . ? C73 C78 H78 118.7 . . ? C106 C101 C102 119.0(6) . . ? C106 C101 H101 120.5 . . ? C102 C101 H101 120.5 . . ? C103 C102 C101 121.4(6) . . ? C103 C102 H102 119.3 . . ? C101 C102 H102 119.3 . . ? C102 C103 C104 118.9(6) . . ? C102 C103 H103 120.5 . . ? C104 C103 H103 120.5 . . ? C105 C104 C103 120.2(6) . . ? C105 C104 H104 119.9 . . ? C103 C104 H104 119.9 . . ? C106 C105 C104 120.1(6) . . ? C106 C105 H105 120 . . ? C104 C105 H105 120 . . ? C101 C106 C105 120.5(6) . . ? C101 C106 H106 119.8 . . ? C105 C106 H106 119.8 . . ? C112 C111 C116 119.7(5) . . ? C112 C111 H111 120.1 . . ? C116 C111 H111 120.1 . . ? C111 C112 C113 120.1(5) . . ? C111 C112 H112 120 . . ? C113 C112 H112 120 . . ? C114 C113 C112 120.0(5) . . ? C114 C113 H113 120 . . ? C112 C113 H113 120 . . ? C113 C114 C115 120.0(5) . . ? C113 C114 H114 120 . . ? C115 C114 H114 120 . . ? C116 C115 C114 119.6(5) . . ? C116 C115 H115 120.2 . . ? C114 C115 H115 120.2 . . ? C115 C116 C111 120.6(5) . . ? C115 C116 H116 119.7 . . ? C111 C116 H116 119.7 . . ? C122 C121 C126 120.3(7) . . ? C122 C121 H121 119.8 . . ? C126 C121 H121 119.8 . . ? C121 C122 C123 120.5(6) . . ? C121 C122 H122 119.7 . . ? C123 C122 H122 119.7 . . ? C124 C123 C122 120.0(7) . . ? C124 C123 H123 120 . . ? C122 C123 H123 120 . . ? C123 C124 C125 120.5(8) . . ? C123 C124 H124 119.8 . . ? C125 C124 H124 119.8 . . ? C124 C125 C126 120.1(7) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? C121 C126 C125 118.4(8) . . ? C121 C126 H126 120.8 . . ? C125 C126 H126 120.8 . . ? C132 C131 C136 118.7(8) . . ? C132 C131 H131 120.7 . . ? C136 C131 H131 120.7 . . ? C131 C132 C133 120.8(9) . . ? C131 C132 H132 119.6 . . ? C133 C132 H132 119.6 . . ? C134 C135 C136 118.2(12) . . ? C134 C135 H135 120.9 . . ? C136 C135 H135 120.9 . . ? C135 C134 C133 122.5(13) . . ? C135 C134 H134 118.8 . . ? C133 C134 H134 118.8 . . ? C134 C133 C132 119.5(11) . . ? C134 C133 H133 120.3 . . ? C132 C133 H133 120.2 . . ? C131 C136 C135 120.4(11) . . ? C131 C136 H136 119.8 . . ? C135 C136 H136 119.8 . . ? 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 C11 S1 Sc1 O1 -54.27(19) . . . . ? C14 S1 Sc1 O1 -147.54(19) . . . . ? C11 S1 Sc1 O2 148.28(19) . . . . ? C14 S1 Sc1 O2 55.02(19) . . . . ? C11 S1 Sc1 N2 47.6(2) . . . . ? C14 S1 Sc1 N2 -45.6(2) . . . . ? C11 S1 Sc1 O3 -129.4(2) . . . . ? C14 S1 Sc1 O3 137.3(2) . . . . ? C11 S1 Sc1 Si4 81.29(17) . . . . ? C14 S1 Sc1 Si4 -11.98(17) . . . . ? O1 Sc1 Si4 N2 19.5(3) . . . . ? O2 Sc1 Si4 N2 -148.3(2) . . . . ? O3 Sc1 Si4 N2 113.4(2) . . . . ? S1 Sc1 Si4 N2 -83.5(2) . . . . ? O1 Sc1 Si4 C4A 123.2(2) . . . . ? O2 Sc1 Si4 C4A -44.6(2) . . . . ? N2 Sc1 Si4 C4A 103.7(3) . . . . ? O3 Sc1 Si4 C4A -142.9(2) . . . . ? S1 Sc1 Si4 C4A 20.17(19) . . . . ? O1 Sc1 Si4 C4B -34.1(3) . . . . ? O2 Sc1 Si4 C4B 158.2(3) . . . . ? N2 Sc1 Si4 C4B -53.5(4) . . . . ? O3 Sc1 Si4 C4B 59.9(3) . . . . ? S1 Sc1 Si4 C4B -137.1(3) . . . . ? O1 Sc1 O2 C22 -77.3(5) . . . . ? N2 Sc1 O2 C22 72.2(5) . . . . ? O3 Sc1 O2 C22 176.2(5) . . . . ? S1 Sc1 O2 C22 -38.7(5) . . . . ? Si4 Sc1 O2 C22 88.4(5) . . . . ? C3A Si3 N2 Si4 70.1(3) . . . . ? C3B Si3 N2 Si4 -51.9(3) . . . . ? C3A Si3 N2 Sc1 -108.4(3) . . . . ? C3B Si3 N2 Sc1 129.6(3) . . . . ? C4A Si4 N2 Si3 91.0(3) . . . . ? C4B Si4 N2 Si3 -31.1(4) . . . . ? Sc1 Si4 N2 Si3 -178.7(4) . . . . ? C4A Si4 N2 Sc1 -90.3(3) . . . . ? C4B Si4 N2 Sc1 147.6(2) . . . . ? O1 Sc1 N2 Si3 12.7(3) . . . . ? O2 Sc1 N2 Si3 -148.9(2) . . . . ? O3 Sc1 N2 Si3 109.3(3) . . . . ? S1 Sc1 N2 Si3 -68.9(3) . . . . ? Si4 Sc1 N2 Si3 178.6(4) . . . . ? O1 Sc1 N2 Si4 -165.97(18) . . . . ? O2 Sc1 N2 Si4 32.4(2) . . . . ? O3 Sc1 N2 Si4 -69.3(2) . . . . ? S1 Sc1 N2 Si4 112.46(18) . . . . ? O1 Sc1 O3 C31 82.9(4) . . . . ? O2 Sc1 O3 C31 -132.1(4) . . . . ? N2 Sc1 O3 C31 -24.4(4) . . . . ? S1 Sc1 O3 C31 152.8(3) . . . . ? Si4 Sc1 O3 C31 -53.0(4) . . . . ? O1 Sc1 O3 C34 -86.3(4) . . . . ? O2 Sc1 O3 C34 58.8(4) . . . . ? N2 Sc1 O3 C34 166.4(4) . . . . ? S1 Sc1 O3 C34 -16.3(5) . . . . ? Si4 Sc1 O3 C34 137.9(4) . . . . ? O2 Sc1 O1 C2 75.2(5) . . . . ? N2 Sc1 O1 C2 -74.2(5) . . . . ? O3 Sc1 O1 C2 -176.8(5) . . . . ? S1 Sc1 O1 C2 36.8(5) . . . . ? Si4 Sc1 O1 C2 -84.4(5) . . . . ? Sc1 O1 C2 C1 -4.7(7) . . . . ? Sc1 O1 C2 C3 173.8(3) . . . . ? C9 C1 C2 O1 173.9(4) . . . . ? C11 C1 C2 O1 -4.0(6) . . . . ? C9 C1 C2 C3 -4.5(7) . . . . ? C11 C1 C2 C3 177.5(4) . . . . ? O1 C2 C3 C4 -173.0(4) . . . . ? C1 C2 C3 C4 5.5(6) . . . . ? O1 C2 C3 Si1 7.7(6) . . . . ? C1 C2 C3 Si1 -173.8(3) . . . . ? C54 Si1 C3 C4 -132.8(4) . . . . ? C41 Si1 C3 C4 -18.0(4) . . . . ? C47 Si1 C3 C4 98.3(4) . . . . ? C54 Si1 C3 C2 46.4(4) . . . . ? C41 Si1 C3 C2 161.2(4) . . . . ? C47 Si1 C3 C2 -82.4(4) . . . . ? C2 C3 C4 C10 -1.2(7) . . . . ? Si1 C3 C4 C10 178.0(3) . . . . ? C10 C5 C6 C7 -2.9(7) . . . . ? C5 C6 C7 C8 2.5(7) . . . . ? C6 C7 C8 C9 0.0(7) . . . . ? C7 C8 C9 C10 -2.1(7) . . . . ? C7 C8 C9 C1 176.2(4) . . . . ? C2 C1 C9 C8 -179.0(4) . . . . ? C11 C1 C9 C8 -1.1(7) . . . . ? C2 C1 C9 C10 -0.7(6) . . . . ? C11 C1 C9 C10 177.1(4) . . . . ? C6 C5 C10 C4 179.2(4) . . . . ? C6 C5 C10 C9 0.8(7) . . . . ? C3 C4 C10 C5 177.6(4) . . . . ? C3 C4 C10 C9 -4.0(7) . . . . ? C8 C9 C10 C5 1.7(6) . . . . ? C1 C9 C10 C5 -176.7(4) . . . . ? C8 C9 C10 C4 -176.8(4) . . . . ? C1 C9 C10 C4 4.9(6) . . . . ? C2 C1 C11 C12 120.0(6) . . . . ? C9 C1 C11 C12 -57.9(7) . . . . ? C2 C1 C11 S1 -53.3(5) . . . . ? C9 C1 C11 S1 128.8(4) . . . . ? C14 S1 C11 C12 -5.5(4) . . . . ? Sc1 S1 C11 C12 -93.8(3) . . . . ? C14 S1 C11 C1 169.3(4) . . . . ? Sc1 S1 C11 C1 81.0(3) . . . . ? C1 C11 C12 C13 -169.1(5) . . . . ? S1 C11 C12 C13 4.6(5) . . . . ? C34 O3 C31 C32 12.0(6) . . . . ? Sc1 O3 C31 C32 -158.8(3) . . . . ? O3 C31 C32 C33 -29.9(6) . . . . ? C31 C32 C33 C34 36.6(6) . . . . ? C31 O3 C34 C33 11.1(6) . . . . ? Sc1 O3 C34 C33 -178.6(3) . . . . ? C32 C33 C34 O3 -29.7(6) . . . . ? C11 C12 C13 C14 -1.0(6) . . . . ? C12 C13 C14 C21 168.9(4) . . . . ? C12 C13 C14 S1 -3.2(5) . . . . ? C11 S1 C14 C13 5.0(4) . . . . ? Sc1 S1 C14 C13 92.7(3) . . . . ? C11 S1 C14 C21 -168.4(4) . . . . ? Sc1 S1 C14 C21 -80.7(3) . . . . ? C13 C14 C21 C22 -119.8(6) . . . . ? S1 C14 C21 C22 51.8(5) . . . . ? C13 C14 C21 C29 57.6(7) . . . . ? S1 C14 C21 C29 -130.8(4) . . . . ? Sc1 O2 C22 C21 6.2(7) . . . . ? Sc1 O2 C22 C23 -170.9(3) . . . . ? C29 C21 C22 O2 -172.9(4) . . . . ? C14 C21 C22 O2 4.5(6) . . . . ? C29 C21 C22 C23 4.1(7) . . . . ? C14 C21 C22 C23 -178.5(4) . . . . ? O2 C22 C23 C24 174.7(4) . . . . ? C21 C22 C23 C24 -2.4(6) . . . . ? O2 C22 C23 Si2 -2.8(6) . . . . ? C21 C22 C23 Si2 -180.0(3) . . . . ? C61 Si2 C23 C24 125.0(4) . . . . ? C67 Si2 C23 C24 -108.4(4) . . . . ? C73 Si2 C23 C24 9.2(4) . . . . ? C61 Si2 C23 C22 -57.5(4) . . . . ? C67 Si2 C23 C22 69.1(4) . . . . ? C73 Si2 C23 C22 -173.3(3) . . . . ? C22 C23 C24 C30 -1.3(7) . . . . ? Si2 C23 C24 C30 176.2(3) . . . . ? C30 C25 C26 C27 0.7(7) . . . . ? C25 C26 C27 C28 0.2(7) . . . . ? C26 C27 C28 C29 -1.4(7) . . . . ? C27 C28 C29 C30 1.6(7) . . . . ? C27 C28 C29 C21 -176.1(4) . . . . ? C22 C21 C29 C28 175.7(4) . . . . ? C14 C21 C29 C28 -1.6(7) . . . . ? C22 C21 C29 C30 -2.1(6) . . . . ? C14 C21 C29 C30 -179.4(4) . . . . ? C26 C25 C30 C29 -0.5(7) . . . . ? C26 C25 C30 C24 178.3(4) . . . . ? C28 C29 C30 C25 -0.7(6) . . . . ? C21 C29 C30 C25 177.2(4) . . . . ? C28 C29 C30 C24 -179.5(4) . . . . ? C21 C29 C30 C24 -1.6(6) . . . . ? C23 C24 C30 C25 -175.4(4) . . . . ? C23 C24 C30 C29 3.4(7) . . . . ? C54 Si1 C41 C42 19.4(4) . . . . ? C3 Si1 C41 C42 -100.2(4) . . . . ? C47 Si1 C41 C42 138.0(4) . . . . ? C54 Si1 C41 C53 -159.6(4) . . . . ? C3 Si1 C41 C53 80.8(4) . . . . ? C47 Si1 C41 C53 -41.0(5) . . . . ? C53 C41 C42 C43 -0.3(7) . . . . ? Si1 C41 C42 C43 -179.4(4) . . . . ? C41 C42 C43 C44 0.5(9) . . . . ? C42 C43 C44 C45 -0.3(9) . . . . ? C43 C44 C45 C53 0.0(8) . . . . ? C54 Si1 C47 C48 71.2(5) . . . . ? C3 Si1 C47 C48 -160.0(4) . . . . ? C41 Si1 C47 C48 -42.1(5) . . . . ? C54 Si1 C47 C52 -111.4(4) . . . . ? C3 Si1 C47 C52 17.4(5) . . . . ? C41 Si1 C47 C52 135.3(4) . . . . ? C52 C47 C48 C49 -1.1(8) . . . . ? Si1 C47 C48 C49 176.5(4) . . . . ? C47 C48 C49 C50 -0.7(8) . . . . ? C48 C49 C50 C51 1.6(9) . . . . ? C49 C50 C51 C52 -0.7(9) . . . . ? C48 C47 C52 C51 1.9(8) . . . . ? Si1 C47 C52 C51 -175.6(4) . . . . ? C50 C51 C52 C47 -1.1(9) . . . . ? C44 C45 C53 C41 0.2(8) . . . . ? C42 C41 C53 C45 0.0(8) . . . . ? Si1 C41 C53 C45 179.0(4) . . . . ? C3 Si1 C54 C59 28.4(5) . . . . ? C41 Si1 C54 C59 -88.4(4) . . . . ? C47 Si1 C54 C59 157.9(4) . . . . ? C3 Si1 C54 C55 -163.1(4) . . . . ? C41 Si1 C54 C55 80.1(4) . . . . ? C47 Si1 C54 C55 -33.5(5) . . . . ? C59 C54 C55 C56 0.0(7) . . . . ? Si1 C54 C55 C56 -168.9(4) . . . . ? C54 C55 C56 C57 0.9(7) . . . . ? C55 C56 C57 C58 -1.2(8) . . . . ? C56 C57 C58 C59 0.7(8) . . . . ? C57 C58 C59 C54 0.2(8) . . . . ? C55 C54 C59 C58 -0.6(7) . . . . ? Si1 C54 C59 C58 168.4(4) . . . . ? C67 Si2 C61 C66 49.9(5) . . . . ? C73 Si2 C61 C66 -67.9(4) . . . . ? C23 Si2 C61 C66 175.4(4) . . . . ? C67 Si2 C61 C62 -129.9(4) . . . . ? C73 Si2 C61 C62 112.3(4) . . . . ? C23 Si2 C61 C62 -4.4(5) . . . . ? C66 C61 C62 C63 0.8(7) . . . . ? Si2 C61 C62 C63 -179.4(4) . . . . ? C61 C62 C63 C64 -1.4(8) . . . . ? C62 C63 C64 C65 0.8(8) . . . . ? C63 C64 C65 C66 0.4(8) . . . . ? C64 C65 C66 C61 -1.0(8) . . . . ? C62 C61 C66 C65 0.4(7) . . . . ? Si2 C61 C66 C65 -179.4(4) . . . . ? C61 Si2 C67 C68 -8.1(5) . . . . ? C73 Si2 C67 C68 108.7(4) . . . . ? C23 Si2 C67 C68 -133.9(4) . . . . ? C61 Si2 C67 C72 174.0(4) . . . . ? C73 Si2 C67 C72 -69.3(4) . . . . ? C23 Si2 C67 C72 48.1(4) . . . . ? C72 C67 C68 C69 0.3(7) . . . . ? Si2 C67 C68 C69 -177.6(4) . . . . ? C67 C68 C69 C70 0.6(8) . . . . ? C68 C69 C70 C71 -1.6(8) . . . . ? C69 C70 C71 C72 1.7(8) . . . . ? C68 C67 C72 C71 -0.3(7) . . . . ? Si2 C67 C72 C71 177.8(4) . . . . ? C70 C71 C72 C67 -0.7(8) . . . . ? C61 Si2 C73 C78 -43.9(4) . . . . ? C67 Si2 C73 C78 -165.0(4) . . . . ? C23 Si2 C73 C78 75.4(4) . . . . ? C61 Si2 C73 C74 133.2(4) . . . . ? C67 Si2 C73 C74 12.1(5) . . . . ? C23 Si2 C73 C74 -107.5(4) . . . . ? C78 C73 C74 C75 1.3(7) . . . . ? Si2 C73 C74 C75 -175.8(4) . . . . ? C73 C74 C75 C76 -0.8(8) . . . . ? C74 C75 C76 C77 -0.8(8) . . . . ? C75 C76 C77 C78 1.6(8) . . . . ? C76 C77 C78 C73 -1.0(9) . . . . ? C74 C73 C78 C77 -0.5(8) . . . . ? Si2 C73 C78 C77 176.9(4) . . . . ? C106 C101 C102 C103 0.2(9) . . . . ? C101 C102 C103 C104 -0.9(9) . . . . ? C102 C103 C104 C105 1.3(9) . . . . ? C103 C104 C105 C106 -1.1(9) . . . . ? C102 C101 C106 C105 0.1(8) . . . . ? C104 C105 C106 C101 0.4(9) . . . . ? C116 C111 C112 C113 0.4(9) . . . . ? C111 C112 C113 C114 0.0(9) . . . . ? C112 C113 C114 C115 -0.4(9) . . . . ? C113 C114 C115 C116 0.3(9) . . . . ? C114 C115 C116 C111 0.2(9) . . . . ? C112 C111 C116 C115 -0.5(9) . . . . ? C126 C121 C122 C123 3.2(10) . . . . ? C121 C122 C123 C124 -2.2(9) . . . . ? C122 C123 C124 C125 1.8(11) . . . . ? C123 C124 C125 C126 -2.2(14) . . . . ? C122 C121 C126 C125 -3.5(12) . . . . ? C124 C125 C126 C121 3.1(15) . . . . ? C136 C131 C132 C133 0.4(11) . . . . ? C136 C135 C134 C133 0(2) . . . . ? C135 C134 C133 C132 0.4(19) . . . . ? C131 C132 C133 C134 -0.8(13) . . . . ? C132 C131 C136 C135 0.5(13) . . . . ? C134 C135 C136 C131 -0.9(18) . . . . ? #===END data_complex9 _database_code_depnum_ccdc_archive 'CCDC 752791' #TrackingRef 'Cif_files_B920283H.cif' _audit_creation_date 2009-11-16T19:01:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C68 H64 La N O3 S Si4, 0.5(C6 H14)' _chemical_formula_sum 'C71 H71 La N O3 S Si4' _chemical_formula_weight 1269.62 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 38.9355(14) _cell_length_b 15.5687(6) _cell_length_c 22.9647(8) _cell_angle_alpha 90 _cell_angle_beta 113.803(2) _cell_angle_gamma 90 _cell_volume 12736.5(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7269 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 26.38 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5256 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 0.891 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_unetI/netI 0.059 _diffrn_reflns_number 67600 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 14447 _reflns_number_gt 10679 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART, 2006' _computing_cell_refinement 'Bruker SMART, 2006' _computing_data_reduction 'Bruker SAINT, 2006' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0372P)^2^+34.0812P] 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_number_reflns 14447 _refine_ls_number_parameters 699 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.09 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.605 _refine_diff_density_min -0.996 _refine_diff_density_rms 0.093 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.859656(5) 0.016576(12) 0.520495(8) 0.02087(6) Uani 1 1 d . A . N2 N 0.87920(8) -0.12703(17) 0.52940(13) 0.0294(6) Uani 1 1 d . A . Si3 Si 0.84579(3) -0.20300(6) 0.49523(4) 0.0267(2) Uani 1 1 d . . . H3S H 0.8098(11) -0.159(2) 0.4748(18) 0.05 Uiso 1 1 d . . . C3A C 0.84776(11) -0.2508(2) 0.42141(16) 0.034 Uani 1 1 d . . . H3A1 H 0.8519 -0.205 0.3956 0.051 Uiso 1 1 calc R . . H3A2 H 0.824 -0.28 0.3967 0.051 Uiso 1 1 calc R . . H3A3 H 0.8684 -0.2922 0.4335 0.051 Uiso 1 1 calc R . . C3B C 0.84621(11) -0.2903(2) 0.55089(17) 0.0363(9) Uani 1 1 d . . . H3B1 H 0.8686 -0.326 0.5607 0.054 Uiso 1 1 calc R . . H3B2 H 0.8237 -0.3257 0.531 0.054 Uiso 1 1 calc R . . H3B3 H 0.8466 -0.265 0.5903 0.054 Uiso 1 1 calc R . . Si4 Si 0.92626(3) -0.13678(7) 0.57202(5) 0.0411(3) Uani 1 1 d . . . H4S H 0.9417(11) -0.050(2) 0.5762(18) 0.05 Uiso 1 1 d . . . C4A1 C 0.9515(2) -0.1862(5) 0.5344(4) 0.041 Uani 0.5 1 d P A 1 H4A1 H 0.9424 -0.2451 0.5229 0.062 Uiso 0.5 1 calc PR A 1 H4A2 H 0.9782 -0.1873 0.5631 0.062 Uiso 0.5 1 calc PR A 1 H4A3 H 0.9483 -0.1541 0.4958 0.062 Uiso 0.5 1 calc PR A 1 C4A2 C 0.9485(2) -0.2297(5) 0.5395(4) 0.041 Uani 0.5 1 d P A 2 H4A4 H 0.9357 -0.284 0.5393 0.062 Uiso 0.5 1 calc PR A 2 H4A5 H 0.9752 -0.2351 0.5669 0.062 Uiso 0.5 1 calc PR A 2 H4A6 H 0.9455 -0.2158 0.496 0.062 Uiso 0.5 1 calc PR A 2 C4B C 0.94006(13) -0.1707(3) 0.65591(19) 0.058 Uani 1 1 d . A . H4B1 H 0.9292 -0.131 0.6771 0.088 Uiso 1 1 calc R . . H4B2 H 0.9675 -0.17 0.678 0.088 Uiso 1 1 calc R . . H4B3 H 0.9308 -0.2289 0.657 0.088 Uiso 1 1 calc R . . O3 O 0.87697(7) 0.03136(14) 0.63632(10) 0.0295(5) Uani 1 1 d . . . C31 C 0.90169(16) 0.0899(3) 0.6816(2) 0.0667(15) Uani 1 1 d . A . H31A H 0.903 0.1446 0.6606 0.08 Uiso 1 1 calc R . . H31B H 0.9273 0.0653 0.7016 0.08 Uiso 1 1 calc R . . C32 C 0.88622(13) 0.1047(3) 0.73032(18) 0.0468(11) Uani 1 1 d . . . H32A H 0.8669 0.1505 0.7168 0.056 Uiso 1 1 calc R A . H32B H 0.9063 0.1203 0.7719 0.056 Uiso 1 1 calc R . . C33 C 0.86915(11) 0.0181(2) 0.73342(16) 0.0371(9) Uani 1 1 d . A . H33A H 0.8476 0.0247 0.7456 0.045 Uiso 1 1 calc R . . H33B H 0.888 -0.0202 0.7644 0.045 Uiso 1 1 calc R . . C34 C 0.85644(13) -0.0167(3) 0.66618(18) 0.0457(10) Uani 1 1 d . A . H34A H 0.8622 -0.0788 0.6671 0.055 Uiso 1 1 calc R . . H34B H 0.8291 -0.0086 0.6425 0.055 Uiso 1 1 calc R . . S1 S 0.81407(2) 0.12980(5) 0.39886(3) 0.01995(16) Uani 1 1 d . . . O1 O 0.90315(6) 0.10893(14) 0.51025(10) 0.0263(5) Uani 1 1 d . . . C1 C 0.88595(9) 0.14479(19) 0.40166(14) 0.0218(7) Uani 1 1 d . . . C2 C 0.90989(9) 0.1523(2) 0.46609(15) 0.0243(7) Uani 1 1 d . A . C3 C 0.94172(9) 0.2087(2) 0.48561(15) 0.0261(7) Uani 1 1 d . . . C4 C 0.94875(9) 0.2528(2) 0.43956(16) 0.0269(7) Uani 1 1 d . A . H4 H 0.9703 0.2887 0.4522 0.032 Uiso 1 1 calc R . . C5 C 0.93203(11) 0.2947(2) 0.32693(17) 0.0331(8) Uani 1 1 d . A . H5 H 0.954 0.329 0.3393 0.04 Uiso 1 1 calc R . . C6 C 0.90770(11) 0.2918(2) 0.26482(18) 0.0379(9) Uani 1 1 d . . . H6 H 0.9126 0.3243 0.234 0.045 Uiso 1 1 calc R . . C7 C 0.87527(11) 0.2406(2) 0.24604(16) 0.0345(8) Uani 1 1 d . A . H7 H 0.8583 0.2393 0.2025 0.041 Uiso 1 1 calc R . . C8 C 0.86774(10) 0.1926(2) 0.28947(15) 0.0287(7) Uani 1 1 d . . . H8 H 0.8456 0.1587 0.2758 0.034 Uiso 1 1 calc R A . C9 C 0.89266(9) 0.19306(19) 0.35459(15) 0.0236(7) Uani 1 1 d . A . C10 C 0.92494(10) 0.2466(2) 0.37389(16) 0.0268(7) Uani 1 1 d . . . C11 C 0.85274(9) 0.08919(19) 0.38736(14) 0.0213(7) Uani 1 1 d . A . C12 C 0.84807(9) 0.00283(19) 0.37490(14) 0.0233(7) Uani 1 1 d . . . H12 H 0.8657 -0.0313 0.3663 0.028 Uiso 1 1 calc R A . C13 C 0.81421(9) -0.03107(19) 0.37600(13) 0.0209(7) Uani 1 1 d . A . H13 H 0.8071 -0.0897 0.3677 0.025 Uiso 1 1 calc R . . C14 C 0.79301(9) 0.02900(18) 0.39013(13) 0.0194(6) Uani 1 1 d . A . Si1 Si 0.97068(3) 0.21893(6) 0.57315(4) 0.0284(2) Uani 1 1 d . A . C41 C 1.00803(14) 0.3023(4) 0.5883(2) 0.0662(6) Uani 1 1 d . . . C42 C 0.99756(15) 0.3884(4) 0.5718(2) 0.0662(6) Uani 1 1 d . A . H42 H 0.9717 0.4017 0.5499 0.079 Uiso 1 1 calc R . . C43 C 1.02353(15) 0.4546(4) 0.5864(2) 0.0662(6) Uani 1 1 d . . . H43 H 1.0159 0.5124 0.575 0.079 Uiso 1 1 calc R A . C44 C 1.06097(14) 0.4330(4) 0.6182(2) 0.0662(6) Uani 1 1 d . A . H44 H 1.0791 0.4777 0.6294 0.079 Uiso 1 1 calc R . . C45 C 1.07318(15) 0.3514(4) 0.6341(2) 0.0662(6) Uani 1 1 d . . . H45 H 1.0992 0.339 0.655 0.079 Uiso 1 1 calc R A . C46 C 1.04626(14) 0.2856(4) 0.6187(2) 0.0662(6) Uani 1 1 d . A . H46 H 1.0544 0.228 0.6294 0.079 Uiso 1 1 calc R . . C47 C 0.99476(10) 0.1138(2) 0.60575(16) 0.0344(8) Uani 1 1 d . . . C48 C 1.01226(13) 0.0705(3) 0.5724(2) 0.0599(14) Uani 1 1 d . A . H48 H 1.0109 0.0937 0.5332 0.072 Uiso 1 1 calc R . . C49 C 1.03163(14) -0.0055(3) 0.5944(3) 0.0748(18) Uani 1 1 d . . . H49 H 1.0431 -0.0336 0.5701 0.09 Uiso 1 1 calc R A . C50 C 1.03439(13) -0.0400(3) 0.6501(3) 0.0705(17) Uani 1 1 d . A . H50 H 1.0481 -0.0917 0.6653 0.085 Uiso 1 1 calc R . . C51 C 1.01711(13) 0.0006(3) 0.6845(2) 0.0581(13) Uani 1 1 d . . . H51 H 1.0186 -0.0235 0.7234 0.07 Uiso 1 1 calc R A . C52 C 0.99745(11) 0.0772(2) 0.66195(18) 0.0412(9) Uani 1 1 d . A . H52 H 0.9857 0.1046 0.686 0.049 Uiso 1 1 calc R . . C53 C 0.94087(10) 0.2605(2) 0.61396(16) 0.0280(7) Uani 1 1 d . . . C54 C 0.95707(12) 0.2771(3) 0.67842(19) 0.0473(11) Uani 1 1 d . A . H54 H 0.983 0.2651 0.7013 0.057 Uiso 1 1 calc R . . C55 C 0.93675(13) 0.3106(3) 0.7112(2) 0.0527(12) Uani 1 1 d . . . H55 H 0.9487 0.3206 0.7558 0.063 Uiso 1 1 calc R A . C56 C 0.89938(13) 0.3291(3) 0.6788(2) 0.0479(11) Uani 1 1 d . A . H56 H 0.8852 0.3507 0.7008 0.057 Uiso 1 1 calc R . . C57 C 0.88272(12) 0.3160(3) 0.6144(2) 0.0490(11) Uani 1 1 d . . . H57 H 0.857 0.3304 0.5916 0.059 Uiso 1 1 calc R A . C58 C 0.90305(11) 0.2818(2) 0.58181(18) 0.0368(9) Uani 1 1 d . A . H58 H 0.891 0.273 0.5372 0.044 Uiso 1 1 calc R . . O2 O 0.79841(6) 0.02882(13) 0.51355(9) 0.0217(5) Uani 1 1 d . . . C21 C 0.75906(9) 0.01870(18) 0.40331(13) 0.0179(6) Uani 1 1 d . . . C22 C 0.76407(9) 0.02206(18) 0.46733(13) 0.0186(6) Uani 1 1 d . A . C23 C 0.73202(9) 0.01756(18) 0.48335(13) 0.0190(6) Uani 1 1 d . . . C24 C 0.69721(9) 0.00553(18) 0.43479(14) 0.0205(6) Uani 1 1 d . A . H24 H 0.6759 0.0029 0.4451 0.025 Uiso 1 1 calc R . . C25 C 0.65568(10) -0.0195(2) 0.32109(15) 0.0273(7) Uani 1 1 d . A . H25 H 0.6346 -0.0256 0.3316 0.033 Uiso 1 1 calc R . . C26 C 0.65110(10) -0.0267(2) 0.25867(16) 0.0326(8) Uani 1 1 d . . . H26 H 0.6269 -0.0379 0.2264 0.039 Uiso 1 1 calc R . . C27 C 0.68212(10) -0.0174(2) 0.24257(15) 0.0297(8) Uani 1 1 d . A . H27 H 0.6787 -0.0217 0.1993 0.036 Uiso 1 1 calc R . . C28 C 0.71715(9) -0.00229(19) 0.28876(14) 0.0221(7) Uani 1 1 d . . . H28 H 0.7379 0.0035 0.2772 0.026 Uiso 1 1 calc R A . C29 C 0.72299(9) 0.00490(17) 0.35382(14) 0.0192(6) Uani 1 1 d . A . C30 C 0.69152(9) -0.00317(18) 0.36980(14) 0.0213(7) Uani 1 1 d . . . Si2 Si 0.73748(3) 0.02284(5) 0.56862(4) 0.01945(18) Uani 1 1 d . A . C61 C 0.76667(9) 0.11668(19) 0.61377(14) 0.0227(7) Uani 1 1 d . . . C62 C 0.77237(9) 0.1879(2) 0.58164(15) 0.0260(7) Uani 1 1 d . A . H62 H 0.7657 0.1846 0.5371 0.031 Uiso 1 1 calc R . . C63 C 0.78763(10) 0.2638(2) 0.61396(17) 0.0314(8) Uani 1 1 d . . . H63 H 0.7907 0.312 0.5911 0.038 Uiso 1 1 calc R A . C64 C 0.79836(10) 0.2693(2) 0.67886(17) 0.0339(8) Uani 1 1 d . A . H64 H 0.8088 0.3212 0.7007 0.041 Uiso 1 1 calc R . . C65 C 0.79391(11) 0.1993(2) 0.71212(16) 0.0376(9) Uani 1 1 d . . . H65 H 0.8017 0.2025 0.757 0.045 Uiso 1 1 calc R A . C66 C 0.77792(10) 0.1240(2) 0.67976(15) 0.0311(8) Uani 1 1 d . A . H66 H 0.7746 0.0765 0.7029 0.037 Uiso 1 1 calc R . . C67 C 0.75328(9) -0.08463(19) 0.60809(14) 0.0223(7) Uani 1 1 d . . . C68 C 0.75106(10) -0.1025(2) 0.66639(15) 0.0302(8) Uani 1 1 d . A . H68 H 0.7431 -0.0586 0.6868 0.036 Uiso 1 1 calc R . . C69 C 0.76018(11) -0.1828(2) 0.69499(17) 0.0370(9) Uani 1 1 d . . . H69 H 0.7591 -0.1928 0.735 0.044 Uiso 1 1 calc R A . C70 C 0.77094(11) -0.2484(2) 0.66489(18) 0.0392(9) Uani 1 1 d . A . H70 H 0.7771 -0.3035 0.6841 0.047 Uiso 1 1 calc R . . C71 C 0.76450(10) -0.1518(2) 0.57934(16) 0.0284(7) Uani 1 1 d . A . H71 H 0.7667 -0.1419 0.5402 0.034 Uiso 1 1 calc R . . C72 C 0.77251(11) -0.2329(2) 0.60701(18) 0.0370(9) Uani 1 1 d . . . H72 H 0.7791 -0.2781 0.5857 0.044 Uiso 1 1 calc R A . C73 C 0.68980(9) 0.04329(19) 0.56886(14) 0.0224(7) Uani 1 1 d . . . C74 C 0.67938(10) 0.1247(2) 0.58183(15) 0.0274(7) Uani 1 1 d . A . H74 H 0.6968 0.1708 0.5915 0.033 Uiso 1 1 calc R . . C75 C 0.64395(11) 0.1387(2) 0.58066(17) 0.0346(8) Uani 1 1 d . . . H75 H 0.6375 0.1942 0.5902 0.041 Uiso 1 1 calc R A . C76 C 0.61800(10) 0.0737(2) 0.56594(17) 0.0328(8) Uani 1 1 d . A . H76 H 0.5936 0.0845 0.5643 0.039 Uiso 1 1 calc R . . C77 C 0.62771(10) -0.0078(2) 0.55340(17) 0.0333(8) Uani 1 1 d . . . H77 H 0.6101 -0.0536 0.5437 0.04 Uiso 1 1 calc R A . C78 C 0.66306(10) -0.0220(2) 0.55508(16) 0.0296(8) Uani 1 1 d . A . H78 H 0.6695 -0.0781 0.5466 0.035 Uiso 1 1 calc R . . C101 C 0.9352(2) 0.5389(5) 0.6148(4) 0.132(3) Uani 0.5 1 d P B 1 H10A H 0.9122 0.5048 0.6019 0.197 Uiso 0.5 1 calc PR B 1 H10B H 0.9512 0.5155 0.5948 0.197 Uiso 0.5 1 calc PR B 1 H10C H 0.9288 0.5986 0.6013 0.197 Uiso 0.5 1 calc PR B 1 C102 C 0.9548(2) 0.5358(6) 0.6824(4) 0.126(3) Uani 0.5 1 d PD B 1 H10D H 0.9465 0.5864 0.6993 0.151 Uiso 0.5 1 calc PR B 1 H10E H 0.9453 0.4846 0.6968 0.151 Uiso 0.5 1 calc PR B 1 C103 C 0.9943(4) 0.5334(16) 0.7141(14) 0.108(7) Uani 0.5 1 d PD . 1 H10F H 1.0053 0.584 0.7018 0.13 Uiso 0.5 1 calc PR . 1 H10G H 1.0041 0.481 0.7015 0.13 Uiso 0.5 1 calc PR . 1 C111 C 0.9352(2) 0.5389(5) 0.6148(4) 0.132(3) Uani 0.5 1 d P C 2 H11A H 0.9092 0.5202 0.6029 0.197 Uiso 0.5 1 calc PR C 2 H11B H 0.9475 0.5009 0.5951 0.197 Uiso 0.5 1 calc PR C 2 H11C H 0.9354 0.5979 0.6 0.197 Uiso 0.5 1 calc PR C 2 C112 C 0.9548(2) 0.5358(6) 0.6824(4) 0.126(3) Uani 0.5 1 d P C 2 H11D H 0.9366 0.5545 0.6999 0.151 Uiso 0.5 1 calc PR C 2 H11E H 0.9598 0.4742 0.6934 0.151 Uiso 0.5 1 calc PR C 2 C113 C 0.9888(5) 0.5794(15) 0.7186(14) 0.108(7) Uani 0.5 1 d PD . 2 H11F H 1.0059 0.5633 0.6979 0.13 Uiso 0.5 1 calc PR . 2 H11G H 0.9828 0.6408 0.7082 0.13 Uiso 0.5 1 calc PR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01947(11) 0.02425(9) 0.02051(9) 0.00140(7) 0.00974(7) 0.00100(8) N2 0.0320(18) 0.0240(14) 0.0303(15) 0.0007(11) 0.0106(13) -0.0011(12) Si3 0.0305(6) 0.0233(4) 0.0290(5) -0.0035(4) 0.0150(4) -0.0002(4) C3A 0.045 0.03 0.033 -0.005 0.021 0 C3B 0.049(3) 0.0298(18) 0.0356(19) -0.0033(15) 0.0234(18) -0.0044(16) Si4 0.0331(7) 0.0393(6) 0.0433(6) 0.0106(5) 0.0075(5) -0.0070(5) C4A1 0.041 0.041 0.041 0 0.017 0 C4A2 0.041 0.041 0.041 0 0.017 0 C4B 0.055 0.062 0.044 0.006 0.005 0.008 O3 0.0314(14) 0.0357(14) 0.0223(11) -0.0001(9) 0.0118(10) -0.0033(10) C31 0.101(4) 0.060(3) 0.049(3) -0.013(2) 0.041(3) -0.029(3) C32 0.069(3) 0.042(2) 0.036(2) -0.0062(17) 0.028(2) -0.005(2) C33 0.042(2) 0.045(2) 0.0282(18) 0.0046(16) 0.0177(17) 0.0021(18) C34 0.063(3) 0.047(2) 0.035(2) -0.0011(18) 0.029(2) -0.014(2) S1 0.0204(4) 0.0210(4) 0.0211(4) -0.0005(3) 0.0110(3) -0.0002(3) O1 0.0230(13) 0.0312(12) 0.0238(11) 0.0008(9) 0.0087(10) -0.0044(10) C1 0.0190(18) 0.0237(15) 0.0272(16) -0.0015(12) 0.0140(14) 0.0008(12) C2 0.0227(19) 0.0244(16) 0.0297(17) 0.0005(13) 0.0148(14) 0.0012(13) C3 0.0220(19) 0.0286(17) 0.0311(17) -0.0025(13) 0.0142(14) -0.0015(13) C4 0.0216(19) 0.0254(16) 0.0391(19) -0.0047(14) 0.0178(15) -0.0032(13) C5 0.038(2) 0.0285(18) 0.045(2) -0.0007(15) 0.0293(18) -0.0013(15) C6 0.052(3) 0.034(2) 0.040(2) 0.0024(16) 0.0315(19) -0.0011(17) C7 0.044(2) 0.0342(19) 0.0290(18) 0.0008(14) 0.0189(17) 0.0008(16) C8 0.032(2) 0.0287(17) 0.0312(17) -0.0010(14) 0.0192(15) -0.0010(14) C9 0.0231(19) 0.0226(15) 0.0302(17) -0.0024(12) 0.0161(14) 0.0025(13) C10 0.026(2) 0.0274(17) 0.0343(18) -0.0023(13) 0.0201(15) 0.0012(14) C11 0.0226(18) 0.0246(16) 0.0197(15) 0.0012(12) 0.0117(13) 0.0010(13) C12 0.0249(19) 0.0297(18) 0.0205(14) -0.0033(12) 0.0144(13) 0.0027(13) C13 0.0244(19) 0.0208(16) 0.0193(14) -0.0022(11) 0.0109(13) -0.0022(12) C14 0.0232(18) 0.0192(15) 0.0162(13) -0.0007(11) 0.0083(12) -0.0020(12) Si1 0.0207(5) 0.0355(5) 0.0300(5) -0.0062(4) 0.0113(4) -0.0039(4) C41 0.0612(14) 0.0956(15) 0.0475(11) -0.0228(11) 0.0279(10) -0.0441(13) C42 0.0612(14) 0.0956(15) 0.0475(11) -0.0228(11) 0.0279(10) -0.0441(13) C43 0.0612(14) 0.0956(15) 0.0475(11) -0.0228(11) 0.0279(10) -0.0441(13) C44 0.0612(14) 0.0956(15) 0.0475(11) -0.0228(11) 0.0279(10) -0.0441(13) C45 0.0612(14) 0.0956(15) 0.0475(11) -0.0228(11) 0.0279(10) -0.0441(13) C46 0.0612(14) 0.0956(15) 0.0475(11) -0.0228(11) 0.0279(10) -0.0441(13) C47 0.020(2) 0.045(2) 0.0316(18) -0.0103(16) 0.0039(15) 0.0033(15) C48 0.046(3) 0.084(3) 0.040(2) -0.016(2) 0.006(2) 0.025(2) C49 0.048(3) 0.086(4) 0.062(3) -0.040(3) -0.007(2) 0.034(3) C50 0.033(3) 0.051(3) 0.087(4) -0.030(3) -0.018(3) 0.018(2) C51 0.038(3) 0.045(3) 0.070(3) 0.005(2) 0.001(2) 0.0035(19) C52 0.030(2) 0.044(2) 0.044(2) -0.0053(17) 0.0087(18) 0.0031(17) C53 0.027(2) 0.0265(17) 0.0325(18) -0.0009(13) 0.0146(15) -0.0006(14) C54 0.031(2) 0.066(3) 0.043(2) -0.019(2) 0.0131(18) 0.0064(19) C55 0.051(3) 0.069(3) 0.044(2) -0.018(2) 0.025(2) 0.006(2) C56 0.057(3) 0.042(2) 0.062(3) -0.0025(19) 0.042(2) 0.012(2) C57 0.035(3) 0.055(3) 0.064(3) 0.007(2) 0.026(2) 0.0189(19) C58 0.034(2) 0.038(2) 0.039(2) 0.0069(16) 0.0156(17) 0.0079(16) O2 0.0204(12) 0.0271(12) 0.0185(10) -0.0005(8) 0.0088(9) -0.0001(9) C21 0.0189(17) 0.0181(13) 0.0206(14) 0.0002(11) 0.0119(12) 0.0004(12) C22 0.0193(17) 0.0166(14) 0.0218(14) 0.0002(11) 0.0103(12) 0.0012(12) C23 0.0226(17) 0.0184(13) 0.0199(14) 0.0015(12) 0.0126(13) 0.0005(12) C24 0.0208(18) 0.0192(15) 0.0260(15) 0.0011(11) 0.0143(13) 0.0007(12) C25 0.0211(19) 0.0325(17) 0.0285(16) 0.0014(14) 0.0103(14) -0.0019(14) C26 0.023(2) 0.043(2) 0.0254(17) -0.0008(15) 0.0034(14) -0.0044(15) C27 0.034(2) 0.0330(17) 0.0208(15) 0.0004(13) 0.0095(14) -0.0014(15) C28 0.0236(19) 0.0244(17) 0.0208(15) 0.0008(11) 0.0116(13) -0.0016(12) C29 0.0219(18) 0.0172(15) 0.0199(14) 0.0005(11) 0.0098(13) -0.0005(11) C30 0.0233(18) 0.0195(16) 0.0226(15) 0.0011(11) 0.0107(13) 0.0000(12) Si2 0.0233(5) 0.0198(4) 0.0198(4) -0.0011(3) 0.0134(3) -0.0007(3) C61 0.0209(18) 0.0240(16) 0.0271(16) -0.0042(12) 0.0138(14) -0.0003(13) C62 0.0253(19) 0.0277(17) 0.0290(17) -0.0011(13) 0.0151(14) 0.0016(14) C63 0.031(2) 0.0220(16) 0.041(2) -0.0006(14) 0.0149(16) 0.0000(14) C64 0.030(2) 0.0250(17) 0.039(2) -0.0118(14) 0.0068(16) 0.0012(14) C65 0.047(3) 0.038(2) 0.0258(18) -0.0082(15) 0.0127(17) -0.0019(17) C66 0.038(2) 0.0302(18) 0.0284(17) -0.0053(14) 0.0174(16) -0.0034(15) C67 0.0244(19) 0.0240(16) 0.0212(15) 0.0010(12) 0.0118(13) -0.0004(13) C68 0.040(2) 0.0280(17) 0.0264(17) -0.0010(13) 0.0170(16) -0.0006(15) C69 0.041(2) 0.038(2) 0.0291(18) 0.0114(15) 0.0111(16) -0.0043(17) C70 0.037(2) 0.0288(19) 0.046(2) 0.0128(16) 0.0112(18) 0.0047(16) C71 0.030(2) 0.0260(17) 0.0328(18) 0.0005(13) 0.0170(15) 0.0018(14) C72 0.037(2) 0.0253(18) 0.052(2) -0.0025(16) 0.0217(19) 0.0044(15) C73 0.0261(19) 0.0240(15) 0.0229(15) 0.0020(12) 0.0159(14) 0.0029(13) C74 0.031(2) 0.0227(16) 0.0329(17) 0.0031(13) 0.0179(15) 0.0019(14) C75 0.040(2) 0.0260(18) 0.046(2) 0.0061(15) 0.0262(18) 0.0122(16) C76 0.026(2) 0.037(2) 0.042(2) 0.0090(15) 0.0209(17) 0.0102(15) C77 0.029(2) 0.0363(19) 0.040(2) -0.0032(15) 0.0195(16) -0.0038(15) C78 0.033(2) 0.0275(17) 0.0364(18) -0.0065(14) 0.0220(16) -0.0017(15) C101 0.121(7) 0.120(6) 0.102(6) -0.011(5) -0.009(5) 0.036(5) C102 0.089(6) 0.151(8) 0.156(8) -0.028(6) 0.067(6) -0.007(5) C103 0.069(7) 0.17(2) 0.089(6) 0.001(15) 0.034(6) -0.006(10) C111 0.121(7) 0.120(6) 0.102(6) -0.011(5) -0.009(5) 0.036(5) C112 0.089(6) 0.151(8) 0.156(8) -0.028(6) 0.067(6) -0.007(5) C113 0.069(7) 0.17(2) 0.089(6) 0.001(15) 0.034(6) -0.006(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O1 2.305(2) . ? La1 O2 2.333(2) . ? La1 N2 2.344(3) . ? La1 O3 2.477(2) . ? La1 C14 3.076(3) . ? La1 S1 3.1715(8) . ? La1 Si4 3.3688(12) . ? La1 Si3 3.4730(9) . ? N2 Si3 1.698(3) . ? N2 Si4 1.700(3) . ? Si3 C3B 1.861(3) . ? Si3 C3A 1.881(3) . ? Si3 H3S 1.45(4) . ? C3A H3A1 0.98 . ? C3A H3A2 0.98 . ? C3A H3A3 0.98 . ? C3B H3B1 0.98 . ? C3B H3B2 0.98 . ? C3B H3B3 0.98 . ? Si4 C4A1 1.730(8) . ? Si4 C4B 1.855(4) . ? Si4 C4A2 1.980(8) . ? Si4 H4S 1.46(4) . ? C4A1 H4A1 0.98 . ? C4A1 H4A2 0.98 . ? C4A1 H4A3 0.98 . ? C4A2 H4A4 0.98 . ? C4A2 H4A5 0.98 . ? C4A2 H4A6 0.98 . ? C4B H4B1 0.98 . ? C4B H4B2 0.98 . ? C4B H4B3 0.98 . ? O3 C31 1.425(5) . ? O3 C34 1.453(4) . ? C31 C32 1.488(6) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.517(5) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 C34 1.519(5) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? S1 C14 1.744(3) . ? S1 C11 1.748(3) . ? O1 C2 1.329(4) . ? C1 C2 1.399(4) . ? C1 C9 1.425(4) . ? C1 C11 1.479(4) . ? C2 C3 1.436(4) . ? C3 C4 1.378(4) . ? C3 Si1 1.873(3) . ? C4 C10 1.420(5) . ? C4 H4 0.95 . ? C5 C6 1.358(5) . ? C5 C10 1.428(5) . ? C5 H5 0.95 . ? C6 C7 1.405(5) . ? C6 H6 0.95 . ? C7 C8 1.369(5) . ? C7 H7 0.95 . ? C8 C9 1.417(4) . ? C8 H8 0.95 . ? C9 C10 1.421(5) . ? C11 C12 1.371(4) . ? C12 C13 1.430(4) . ? C12 H12 0.95 . ? C13 C14 1.370(4) . ? C13 H13 0.95 . ? C14 C21 1.479(4) . ? Si1 C41 1.874(5) . ? Si1 C53 1.877(4) . ? Si1 C47 1.884(4) . ? C41 C46 1.390(7) . ? C41 C42 1.409(8) . ? C42 C43 1.387(6) . ? C42 H42 0.95 . ? C43 C44 1.383(7) . ? C43 H43 0.95 . ? C44 C45 1.353(7) . ? C44 H44 0.95 . ? C45 C46 1.405(6) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? C47 C52 1.376(5) . ? C47 C48 1.389(5) . ? C48 C49 1.384(7) . ? C48 H48 0.95 . ? C49 C50 1.350(8) . ? C49 H49 0.95 . ? C50 C51 1.381(7) . ? C50 H50 0.95 . ? C51 C52 1.399(5) . ? C51 H51 0.95 . ? C52 H52 0.95 . ? C53 C54 1.379(5) . ? C53 C58 1.395(5) . ? C54 C55 1.396(5) . ? C54 H54 0.95 . ? C55 C56 1.371(6) . ? C55 H55 0.95 . ? C56 C57 1.369(6) . ? C56 H56 0.95 . ? C57 C58 1.395(5) . ? C57 H57 0.95 . ? C58 H58 0.95 . ? O2 C22 1.334(4) . ? C21 C22 1.404(4) . ? C21 C29 1.422(4) . ? C22 C23 1.438(4) . ? C23 C24 1.377(4) . ? C23 Si2 1.884(3) . ? C24 C30 1.424(4) . ? C24 H24 0.95 . ? C25 C26 1.376(5) . ? C25 C30 1.415(4) . ? C25 H25 0.95 . ? C26 C27 1.406(5) . ? C26 H26 0.95 . ? C27 C28 1.369(5) . ? C27 H27 0.95 . ? C28 C29 1.422(4) . ? C28 H28 0.95 . ? C29 C30 1.420(5) . ? Si2 C67 1.884(3) . ? Si2 C61 1.884(3) . ? Si2 C73 1.886(3) . ? C61 C62 1.399(4) . ? C61 C66 1.402(4) . ? C62 C63 1.394(4) . ? C62 H62 0.95 . ? C63 C64 1.379(5) . ? C63 H63 0.95 . ? C64 C65 1.382(5) . ? C64 H64 0.95 . ? C65 C66 1.393(5) . ? C65 H65 0.95 . ? C66 H66 0.95 . ? C67 C71 1.398(4) . ? C67 C68 1.404(4) . ? C68 C69 1.389(5) . ? C68 H68 0.95 . ? C69 C70 1.390(5) . ? C69 H69 0.95 . ? C70 C72 1.377(5) . ? C70 H70 0.95 . ? C71 C72 1.391(5) . ? C71 H71 0.95 . ? C72 H72 0.95 . ? C73 C78 1.397(5) . ? C73 C74 1.398(4) . ? C74 C75 1.386(5) . ? C74 H74 0.95 . ? C75 C76 1.372(5) . ? C75 H75 0.95 . ? C76 C77 1.388(5) . ? C76 H76 0.95 . ? C77 C78 1.379(5) . ? C77 H77 0.95 . ? C78 H78 0.95 . ? C101 C102 1.428(10) . ? C101 H10A 0.98 . ? C101 H10B 0.98 . ? C101 H10C 0.98 . ? C102 C103 1.411(16) . ? C102 H10D 0.99 . ? C102 H10E 0.99 . ? C103 C103 1.53(6) 2_756 ? C103 H10F 0.99 . ? C103 H10G 0.99 . ? C113 C113 1.35(5) 2_756 ? C113 H11F 0.99 . ? C113 H11G 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 La1 O2 135.64(7) . . ? O1 La1 N2 112.21(9) . . ? O2 La1 N2 111.77(9) . . ? O1 La1 O3 99.15(7) . . ? O2 La1 O3 83.88(7) . . ? N2 La1 O3 93.26(8) . . ? O1 La1 C14 103.14(8) . . ? O2 La1 C14 59.39(8) . . ? N2 La1 C14 105.16(8) . . ? O3 La1 C14 142.78(8) . . ? O1 La1 S1 74.72(5) . . ? O2 La1 S1 72.61(5) . . ? N2 La1 S1 130.81(7) . . ? O3 La1 S1 135.01(6) . . ? C14 La1 S1 32.38(5) . . ? O1 La1 Si4 89.13(6) . . ? O2 La1 Si4 134.64(5) . . ? N2 La1 Si4 27.94(7) . . ? O3 La1 Si4 81.46(6) . . ? C14 La1 Si4 127.87(6) . . ? S1 La1 Si4 141.36(2) . . ? O1 La1 Si3 131.92(6) . . ? O2 La1 Si3 89.04(5) . . ? N2 La1 Si3 25.68(7) . . ? O3 La1 Si3 103.15(5) . . ? C14 La1 Si3 83.46(5) . . ? S1 La1 Si3 113.95(2) . . ? Si4 La1 Si3 53.61(2) . . ? Si3 N2 Si4 130.58(17) . . ? Si3 N2 La1 117.58(15) . . ? Si4 N2 La1 111.83(14) . . ? N2 Si3 C3B 113.48(15) . . ? N2 Si3 C3A 112.93(16) . . ? C3B Si3 C3A 109.76(16) . . ? C3B Si3 La1 130.25(11) . . ? C3A Si3 La1 118.66(11) . . ? N2 Si3 H3S 106.4(15) . . ? C3B Si3 H3S 107.7(15) . . ? C3A Si3 H3S 106.1(15) . . ? La1 Si3 H3S 70.0(15) . . ? Si3 C3A H3A1 109.5 . . ? Si3 C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? Si3 C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? Si3 C3B H3B1 109.5 . . ? Si3 C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? Si3 C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? N2 Si4 C4A1 116.7(3) . . ? N2 Si4 C4B 114.61(19) . . ? C4A1 Si4 C4B 114.1(3) . . ? N2 Si4 C4A2 112.4(3) . . ? C4B Si4 C4A2 101.4(3) . . ? C4A1 Si4 La1 130.7(3) . . ? C4B Si4 La1 115.18(16) . . ? C4A2 Si4 La1 141.0(2) . . ? N2 Si4 H4S 105.9(15) . . ? C4A1 Si4 H4S 98.1(15) . . ? C4B Si4 H4S 104.8(15) . . ? C4A2 Si4 H4S 117.8(15) . . ? La1 Si4 H4S 66.9(15) . . ? Si4 C4A1 H4A1 109.5 . . ? Si4 C4A1 H4A2 109.5 . . ? Si4 C4A1 H4A3 109.5 . . ? Si4 C4A2 H4A4 109.5 . . ? Si4 C4A2 H4A5 109.5 . . ? H4A4 C4A2 H4A5 109.5 . . ? Si4 C4A2 H4A6 109.5 . . ? H4A4 C4A2 H4A6 109.5 . . ? H4A5 C4A2 H4A6 109.5 . . ? Si4 C4B H4B1 109.5 . . ? Si4 C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? Si4 C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C31 O3 C34 108.9(3) . . ? C31 O3 La1 130.8(2) . . ? C34 O3 La1 119.7(2) . . ? O3 C31 C32 106.8(4) . . ? O3 C31 H31A 110.4 . . ? C32 C31 H31A 110.4 . . ? O3 C31 H31B 110.4 . . ? C32 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? C31 C32 C33 102.5(3) . . ? C31 C32 H32A 111.3 . . ? C33 C32 H32A 111.3 . . ? C31 C32 H32B 111.3 . . ? C33 C32 H32B 111.3 . . ? H32A C32 H32B 109.2 . . ? C32 C33 C34 103.8(3) . . ? C32 C33 H33A 111 . . ? C34 C33 H33A 111 . . ? C32 C33 H33B 111 . . ? C34 C33 H33B 111 . . ? H33A C33 H33B 109 . . ? O3 C34 C33 106.3(3) . . ? O3 C34 H34A 110.5 . . ? C33 C34 H34A 110.5 . . ? O3 C34 H34B 110.5 . . ? C33 C34 H34B 110.5 . . ? H34A C34 H34B 108.7 . . ? C14 S1 C11 92.91(15) . . ? C14 S1 La1 70.80(10) . . ? C11 S1 La1 73.86(10) . . ? C2 O1 La1 140.71(19) . . ? C2 C1 C9 120.7(3) . . ? C2 C1 C11 115.7(3) . . ? C9 C1 C11 123.5(3) . . ? O1 C2 C1 120.8(3) . . ? O1 C2 C3 118.9(3) . . ? C1 C2 C3 120.3(3) . . ? C4 C3 C2 118.7(3) . . ? C4 C3 Si1 124.1(3) . . ? C2 C3 Si1 117.2(2) . . ? C3 C4 C10 122.3(3) . . ? C3 C4 H4 118.9 . . ? C10 C4 H4 118.9 . . ? C6 C5 C10 120.7(3) . . ? C6 C5 H5 119.7 . . ? C10 C5 H5 119.7 . . ? C5 C6 C7 120.0(3) . . ? C5 C6 H6 120 . . ? C7 C6 H6 120 . . ? C8 C7 C6 121.0(3) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 120.6(3) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 118.4(3) . . ? C8 C9 C1 122.8(3) . . ? C10 C9 C1 118.8(3) . . ? C4 C10 C9 119.2(3) . . ? C4 C10 C5 121.6(3) . . ? C9 C10 C5 119.2(3) . . ? C12 C11 C1 130.6(3) . . ? C12 C11 S1 109.7(2) . . ? C1 C11 S1 118.9(2) . . ? C11 C12 C13 113.8(3) . . ? C11 C12 H12 123.1 . . ? C13 C12 H12 123.1 . . ? C14 C13 C12 113.6(3) . . ? C14 C13 H13 123.2 . . ? C12 C13 H13 123.2 . . ? C13 C14 C21 130.4(3) . . ? C13 C14 S1 109.9(2) . . ? C21 C14 S1 119.4(2) . . ? C13 C14 La1 80.53(18) . . ? C21 C14 La1 105.46(17) . . ? S1 C14 La1 76.82(10) . . ? C3 Si1 C41 110.11(18) . . ? C3 Si1 C53 109.85(15) . . ? C41 Si1 C53 105.0(2) . . ? C3 Si1 C47 109.88(15) . . ? C41 Si1 C47 107.7(2) . . ? C53 Si1 C47 114.21(16) . . ? C46 C41 C42 116.6(4) . . ? C46 C41 Si1 123.9(4) . . ? C42 C41 Si1 119.4(4) . . ? C43 C42 C41 122.6(5) . . ? C43 C42 H42 118.7 . . ? C41 C42 H42 118.7 . . ? C44 C43 C42 117.2(6) . . ? C44 C43 H43 121.4 . . ? C42 C43 H43 121.4 . . ? C45 C44 C43 123.5(5) . . ? C45 C44 H44 118.3 . . ? C43 C44 H44 118.3 . . ? C44 C45 C46 118.1(5) . . ? C44 C45 H45 120.9 . . ? C46 C45 H45 120.9 . . ? C41 C46 C45 121.9(6) . . ? C41 C46 H46 119 . . ? C45 C46 H46 119 . . ? C52 C47 C48 116.6(4) . . ? C52 C47 Si1 124.7(3) . . ? C48 C47 Si1 118.6(3) . . ? C49 C48 C47 122.0(5) . . ? C49 C48 H48 119 . . ? C47 C48 H48 119 . . ? C50 C49 C48 120.7(5) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C49 C50 C51 119.2(4) . . ? C49 C50 H50 120.4 . . ? C51 C50 H50 120.4 . . ? C50 C51 C52 120.0(5) . . ? C50 C51 H51 120 . . ? C52 C51 H51 120 . . ? C47 C52 C51 121.6(4) . . ? C47 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C54 C53 C58 116.8(3) . . ? C54 C53 Si1 119.6(3) . . ? C58 C53 Si1 123.5(3) . . ? C53 C54 C55 122.4(4) . . ? C53 C54 H54 118.8 . . ? C55 C54 H54 118.8 . . ? C56 C55 C54 119.5(4) . . ? C56 C55 H55 120.2 . . ? C54 C55 H55 120.2 . . ? C57 C56 C55 119.5(4) . . ? C57 C56 H56 120.2 . . ? C55 C56 H56 120.2 . . ? C56 C57 C58 120.8(4) . . ? C56 C57 H57 119.6 . . ? C58 C57 H57 119.6 . . ? C53 C58 C57 120.9(4) . . ? C53 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? C22 O2 La1 135.77(18) . . ? C22 C21 C29 121.2(3) . . ? C22 C21 C14 116.9(3) . . ? C29 C21 C14 121.9(3) . . ? O2 C22 C21 120.5(3) . . ? O2 C22 C23 119.7(2) . . ? C21 C22 C23 119.9(3) . . ? C24 C23 C22 118.1(3) . . ? C24 C23 Si2 120.6(2) . . ? C22 C23 Si2 121.2(2) . . ? C23 C24 C30 123.2(3) . . ? C23 C24 H24 118.4 . . ? C30 C24 H24 118.4 . . ? C26 C25 C30 120.7(3) . . ? C26 C25 H25 119.7 . . ? C30 C25 H25 119.7 . . ? C25 C26 C27 120.1(3) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 120.5(3) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 121.0(3) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C30 C29 C21 118.9(3) . . ? C30 C29 C28 118.4(3) . . ? C21 C29 C28 122.6(3) . . ? C25 C30 C29 119.3(3) . . ? C25 C30 C24 122.1(3) . . ? C29 C30 C24 118.5(3) . . ? C67 Si2 C61 114.62(14) . . ? C67 Si2 C23 109.83(13) . . ? C61 Si2 C23 113.31(14) . . ? C67 Si2 C73 106.21(14) . . ? C61 Si2 C73 104.08(14) . . ? C23 Si2 C73 108.18(14) . . ? C62 C61 C66 117.3(3) . . ? C62 C61 Si2 120.9(2) . . ? C66 C61 Si2 120.9(2) . . ? C63 C62 C61 121.0(3) . . ? C63 C62 H62 119.5 . . ? C61 C62 H62 119.5 . . ? C64 C63 C62 120.4(3) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 C65 119.8(3) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C64 C65 C66 119.9(3) . . ? C64 C65 H65 120.1 . . ? C66 C65 H65 120.1 . . ? C65 C66 C61 121.5(3) . . ? C65 C66 H66 119.3 . . ? C61 C66 H66 119.3 . . ? C71 C67 C68 116.9(3) . . ? C71 C67 Si2 122.7(2) . . ? C68 C67 Si2 120.1(2) . . ? C69 C68 C67 121.8(3) . . ? C69 C68 H68 119.1 . . ? C67 C68 H68 119.1 . . ? C68 C69 C70 119.8(3) . . ? C68 C69 H69 120.1 . . ? C70 C69 H69 120.1 . . ? C72 C70 C69 119.4(3) . . ? C72 C70 H70 120.3 . . ? C69 C70 H70 120.3 . . ? C72 C71 C67 121.2(3) . . ? C72 C71 H71 119.4 . . ? C67 C71 H71 119.4 . . ? C70 C72 C71 120.8(3) . . ? C70 C72 H72 119.6 . . ? C71 C72 H72 119.6 . . ? C78 C73 C74 117.0(3) . . ? C78 C73 Si2 121.4(2) . . ? C74 C73 Si2 121.6(3) . . ? C75 C74 C73 120.7(3) . . ? C75 C74 H74 119.6 . . ? C73 C74 H74 119.6 . . ? C76 C75 C74 121.1(3) . . ? C76 C75 H75 119.4 . . ? C74 C75 H75 119.4 . . ? C75 C76 C77 119.4(3) . . ? C75 C76 H76 120.3 . . ? C77 C76 H76 120.3 . . ? C78 C77 C76 119.5(3) . . ? C78 C77 H77 120.2 . . ? C76 C77 H77 120.2 . . ? C77 C78 C73 122.3(3) . . ? C77 C78 H78 118.8 . . ? C73 C78 H78 118.8 . . ? C102 C101 H10A 109.5 . . ? C102 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C102 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C103 C102 C101 123.7(15) . . ? C103 C102 H10D 106.4 . . ? C101 C102 H10D 106.4 . . ? C103 C102 H10E 106.4 . . ? C101 C102 H10E 106.4 . . ? H10D C102 H10E 106.5 . . ? C102 C103 C103 110(2) . 2_756 ? C102 C103 H10F 109.7 . . ? C103 C103 H10F 109.7 2_756 . ? C102 C103 H10G 109.7 . . ? C103 C103 H10G 109.7 2_756 . ? H10F C103 H10G 108.2 . . ? C113 C113 H11F 104.2 2_756 . ? C113 C113 H11G 104.2 2_756 . ? H11F C113 H11G 105.5 . . ? 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 O1 La1 N2 Si3 -144.72(14) . . . . ? O2 La1 N2 Si3 29.32(18) . . . . ? O3 La1 N2 Si3 114.03(15) . . . . ? C14 La1 N2 Si3 -33.31(17) . . . . ? S1 La1 N2 Si3 -56.07(19) . . . . ? Si4 La1 N2 Si3 178.9(3) . . . . ? O1 La1 N2 Si4 36.42(17) . . . . ? O2 La1 N2 Si4 -149.55(13) . . . . ? O3 La1 N2 Si4 -64.84(15) . . . . ? C14 La1 N2 Si4 147.83(14) . . . . ? S1 La1 N2 Si4 125.07(11) . . . . ? Si3 La1 N2 Si4 -178.9(3) . . . . ? Si4 N2 Si3 C3B 52.0(3) . . . . ? La1 N2 Si3 C3B -126.57(17) . . . . ? Si4 N2 Si3 C3A -73.7(3) . . . . ? La1 N2 Si3 C3A 107.69(18) . . . . ? Si4 N2 Si3 La1 178.6(3) . . . . ? O1 La1 Si3 N2 45.95(18) . . . . ? O2 La1 Si3 N2 -152.95(17) . . . . ? O3 La1 Si3 N2 -69.46(17) . . . . ? C14 La1 Si3 N2 147.76(17) . . . . ? S1 La1 Si3 N2 136.59(16) . . . . ? Si4 La1 Si3 N2 -0.66(16) . . . . ? O1 La1 Si3 C3B 120.79(19) . . . . ? O2 La1 Si3 C3B -78.11(18) . . . . ? N2 La1 Si3 C3B 74.8(2) . . . . ? O3 La1 Si3 C3B 5.38(18) . . . . ? C14 La1 Si3 C3B -137.40(18) . . . . ? S1 La1 Si3 C3B -148.57(17) . . . . ? Si4 La1 Si3 C3B 74.18(17) . . . . ? O1 La1 Si3 C3A -44.62(16) . . . . ? O2 La1 Si3 C3A 116.48(15) . . . . ? N2 La1 Si3 C3A -90.6(2) . . . . ? O3 La1 Si3 C3A -160.03(15) . . . . ? C14 La1 Si3 C3A 57.19(15) . . . . ? S1 La1 Si3 C3A 46.02(15) . . . . ? Si4 La1 Si3 C3A -91.23(15) . . . . ? Si3 N2 Si4 C4A1 59.0(4) . . . . ? La1 N2 Si4 C4A1 -122.3(3) . . . . ? Si3 N2 Si4 C4B -78.1(3) . . . . ? La1 N2 Si4 C4B 100.6(2) . . . . ? Si3 N2 Si4 C4A2 36.9(4) . . . . ? La1 N2 Si4 C4A2 -144.4(3) . . . . ? Si3 N2 Si4 La1 -178.7(3) . . . . ? O1 La1 Si4 N2 -146.65(16) . . . . ? O2 La1 Si4 N2 41.42(17) . . . . ? O3 La1 Si4 N2 113.97(16) . . . . ? C14 La1 Si4 N2 -40.61(17) . . . . ? S1 La1 Si4 N2 -82.83(15) . . . . ? Si3 La1 Si4 N2 0.61(15) . . . . ? O1 La1 Si4 C4A1 -62.2(4) . . . . ? O2 La1 Si4 C4A1 125.8(4) . . . . ? N2 La1 Si4 C4A1 84.4(4) . . . . ? O3 La1 Si4 C4A1 -161.6(4) . . . . ? C14 La1 Si4 C4A1 43.8(4) . . . . ? S1 La1 Si4 C4A1 1.6(4) . . . . ? Si3 La1 Si4 C4A1 85.0(4) . . . . ? O1 La1 Si4 C4B 114.34(18) . . . . ? O2 La1 Si4 C4B -57.59(19) . . . . ? N2 La1 Si4 C4B -99.0(2) . . . . ? O3 La1 Si4 C4B 14.96(18) . . . . ? C14 La1 Si4 C4B -139.63(19) . . . . ? S1 La1 Si4 C4B 178.16(17) . . . . ? Si3 La1 Si4 C4B -98.40(18) . . . . ? O1 La1 Si4 C4A2 -88.0(4) . . . . ? O2 La1 Si4 C4A2 100.1(4) . . . . ? N2 La1 Si4 C4A2 58.7(4) . . . . ? O3 La1 Si4 C4A2 172.6(4) . . . . ? C14 La1 Si4 C4A2 18.1(4) . . . . ? S1 La1 Si4 C4A2 -24.2(4) . . . . ? Si3 La1 Si4 C4A2 59.3(4) . . . . ? O1 La1 O3 C31 9.7(4) . . . . ? O2 La1 O3 C31 -125.6(4) . . . . ? N2 La1 O3 C31 122.8(4) . . . . ? C14 La1 O3 C31 -116.7(4) . . . . ? S1 La1 O3 C31 -67.8(4) . . . . ? Si4 La1 O3 C31 97.4(4) . . . . ? Si3 La1 O3 C31 146.8(4) . . . . ? O1 La1 O3 C34 180.0(3) . . . . ? O2 La1 O3 C34 44.6(3) . . . . ? N2 La1 O3 C34 -66.9(3) . . . . ? C14 La1 O3 C34 53.6(3) . . . . ? S1 La1 O3 C34 102.5(3) . . . . ? Si4 La1 O3 C34 -92.3(3) . . . . ? Si3 La1 O3 C34 -42.9(3) . . . . ? C34 O3 C31 C32 -22.8(5) . . . . ? La1 O3 C31 C32 148.3(3) . . . . ? O3 C31 C32 C33 33.9(5) . . . . ? C31 C32 C33 C34 -31.6(5) . . . . ? C31 O3 C34 C33 1.9(5) . . . . ? La1 O3 C34 C33 -170.3(2) . . . . ? C32 C33 C34 O3 19.0(4) . . . . ? O1 La1 S1 C14 150.58(12) . . . . ? O2 La1 S1 C14 -59.84(12) . . . . ? N2 La1 S1 C14 44.22(15) . . . . ? O3 La1 S1 C14 -121.72(13) . . . . ? Si4 La1 S1 C14 82.11(12) . . . . ? Si3 La1 S1 C14 21.05(11) . . . . ? O1 La1 S1 C11 51.56(12) . . . . ? O2 La1 S1 C11 -158.86(12) . . . . ? N2 La1 S1 C11 -54.80(14) . . . . ? O3 La1 S1 C11 139.26(13) . . . . ? C14 La1 S1 C11 -99.02(15) . . . . ? Si4 La1 S1 C11 -16.91(12) . . . . ? Si3 La1 S1 C11 -77.97(11) . . . . ? O2 La1 O1 C2 -72.1(3) . . . . ? N2 La1 O1 C2 99.9(3) . . . . ? O3 La1 O1 C2 -162.7(3) . . . . ? C14 La1 O1 C2 -12.7(3) . . . . ? S1 La1 O1 C2 -28.4(3) . . . . ? Si4 La1 O1 C2 116.1(3) . . . . ? Si3 La1 O1 C2 80.3(3) . . . . ? La1 O1 C2 C1 -2.6(5) . . . . ? La1 O1 C2 C3 176.0(2) . . . . ? C9 C1 C2 O1 178.3(3) . . . . ? C11 C1 C2 O1 2.3(4) . . . . ? C9 C1 C2 C3 -0.2(5) . . . . ? C11 C1 C2 C3 -176.2(3) . . . . ? O1 C2 C3 C4 179.4(3) . . . . ? C1 C2 C3 C4 -2.1(5) . . . . ? O1 C2 C3 Si1 -1.7(4) . . . . ? C1 C2 C3 Si1 176.8(2) . . . . ? C2 C3 C4 C10 2.2(5) . . . . ? Si1 C3 C4 C10 -176.6(2) . . . . ? C10 C5 C6 C7 -0.4(5) . . . . ? C5 C6 C7 C8 -0.5(6) . . . . ? C6 C7 C8 C9 -0.3(5) . . . . ? C7 C8 C9 C10 2.0(5) . . . . ? C7 C8 C9 C1 179.5(3) . . . . ? C2 C1 C9 C8 -175.1(3) . . . . ? C11 C1 C9 C8 0.6(5) . . . . ? C2 C1 C9 C10 2.4(5) . . . . ? C11 C1 C9 C10 178.1(3) . . . . ? C3 C4 C10 C9 0.0(5) . . . . ? C3 C4 C10 C5 178.2(3) . . . . ? C8 C9 C10 C4 175.4(3) . . . . ? C1 C9 C10 C4 -2.3(4) . . . . ? C8 C9 C10 C5 -2.8(5) . . . . ? C1 C9 C10 C5 179.5(3) . . . . ? C6 C5 C10 C4 -176.0(3) . . . . ? C6 C5 C10 C9 2.1(5) . . . . ? C2 C1 C11 C12 -89.7(4) . . . . ? C9 C1 C11 C12 94.4(4) . . . . ? C2 C1 C11 S1 78.8(3) . . . . ? C9 C1 C11 S1 -97.1(3) . . . . ? C14 S1 C11 C12 2.4(2) . . . . ? La1 S1 C11 C12 71.5(2) . . . . ? C14 S1 C11 C1 -168.4(2) . . . . ? La1 S1 C11 C1 -99.3(2) . . . . ? C1 C11 C12 C13 168.0(3) . . . . ? S1 C11 C12 C13 -1.4(3) . . . . ? C11 C12 C13 C14 -0.8(4) . . . . ? C12 C13 C14 C21 -171.9(3) . . . . ? C12 C13 C14 S1 2.6(3) . . . . ? C12 C13 C14 La1 -69.6(2) . . . . ? C11 S1 C14 C13 -2.8(2) . . . . ? La1 S1 C14 C13 -74.6(2) . . . . ? C11 S1 C14 C21 172.3(2) . . . . ? La1 S1 C14 C21 100.5(2) . . . . ? C11 S1 C14 La1 71.80(10) . . . . ? O1 La1 C14 C13 84.11(18) . . . . ? O2 La1 C14 C13 -140.2(2) . . . . ? N2 La1 C14 C13 -33.6(2) . . . . ? O3 La1 C14 C13 -150.64(17) . . . . ? S1 La1 C14 C13 113.2(2) . . . . ? Si4 La1 C14 C13 -15.2(2) . . . . ? Si3 La1 C14 C13 -47.48(17) . . . . ? O1 La1 C14 C21 -146.44(17) . . . . ? O2 La1 C14 C21 -10.80(16) . . . . ? N2 La1 C14 C21 95.83(19) . . . . ? O3 La1 C14 C21 -21.2(2) . . . . ? S1 La1 C14 C21 -117.3(2) . . . . ? Si4 La1 C14 C21 114.25(17) . . . . ? Si3 La1 C14 C21 81.97(17) . . . . ? O1 La1 C14 S1 -29.11(12) . . . . ? O2 La1 C14 S1 106.53(12) . . . . ? N2 La1 C14 S1 -146.84(11) . . . . ? O3 La1 C14 S1 96.14(14) . . . . ? Si4 La1 C14 S1 -128.42(8) . . . . ? Si3 La1 C14 S1 -160.70(10) . . . . ? C4 C3 Si1 C41 3.7(4) . . . . ? C2 C3 Si1 C41 -175.2(3) . . . . ? C4 C3 Si1 C53 118.8(3) . . . . ? C2 C3 Si1 C53 -60.0(3) . . . . ? C4 C3 Si1 C47 -114.8(3) . . . . ? C2 C3 Si1 C47 66.4(3) . . . . ? C3 Si1 C41 C46 -120.1(4) . . . . ? C53 Si1 C41 C46 121.8(4) . . . . ? C47 Si1 C41 C46 -0.3(4) . . . . ? C3 Si1 C41 C42 64.0(4) . . . . ? C53 Si1 C41 C42 -54.2(4) . . . . ? C47 Si1 C41 C42 -176.3(3) . . . . ? C46 C41 C42 C43 -1.8(7) . . . . ? Si1 C41 C42 C43 174.5(3) . . . . ? C41 C42 C43 C44 0.2(7) . . . . ? C42 C43 C44 C45 1.5(7) . . . . ? C43 C44 C45 C46 -1.5(7) . . . . ? C42 C41 C46 C45 1.8(7) . . . . ? Si1 C41 C46 C45 -174.3(3) . . . . ? C44 C45 C46 C41 -0.3(7) . . . . ? C3 Si1 C47 C52 -136.7(3) . . . . ? C41 Si1 C47 C52 103.3(4) . . . . ? C53 Si1 C47 C52 -12.8(4) . . . . ? C3 Si1 C47 C48 45.4(4) . . . . ? C41 Si1 C47 C48 -74.5(4) . . . . ? C53 Si1 C47 C48 169.4(3) . . . . ? C52 C47 C48 C49 -0.3(7) . . . . ? Si1 C47 C48 C49 177.7(4) . . . . ? C47 C48 C49 C50 -0.5(8) . . . . ? C48 C49 C50 C51 1.0(8) . . . . ? C49 C50 C51 C52 -0.8(7) . . . . ? C48 C47 C52 C51 0.5(6) . . . . ? Si1 C47 C52 C51 -177.3(3) . . . . ? C50 C51 C52 C47 0.0(6) . . . . ? C3 Si1 C53 C54 -176.8(3) . . . . ? C41 Si1 C53 C54 -58.4(4) . . . . ? C47 Si1 C53 C54 59.3(3) . . . . ? C3 Si1 C53 C58 -1.4(3) . . . . ? C41 Si1 C53 C58 117.0(3) . . . . ? C47 Si1 C53 C58 -125.4(3) . . . . ? C58 C53 C54 C55 2.2(6) . . . . ? Si1 C53 C54 C55 177.9(3) . . . . ? C53 C54 C55 C56 -0.7(7) . . . . ? C54 C55 C56 C57 -1.4(7) . . . . ? C55 C56 C57 C58 1.9(7) . . . . ? C54 C53 C58 C57 -1.7(5) . . . . ? Si1 C53 C58 C57 -177.2(3) . . . . ? C56 C57 C58 C53 -0.3(6) . . . . ? O1 La1 O2 C22 89.7(3) . . . . ? N2 La1 O2 C22 -82.4(3) . . . . ? O3 La1 O2 C22 -173.5(3) . . . . ? C14 La1 O2 C22 12.8(2) . . . . ? S1 La1 O2 C22 45.4(2) . . . . ? Si4 La1 O2 C22 -101.9(2) . . . . ? Si3 La1 O2 C22 -70.1(2) . . . . ? C13 C14 C21 C22 101.7(4) . . . . ? S1 C14 C21 C22 -72.3(3) . . . . ? La1 C14 C21 C22 11.1(3) . . . . ? C13 C14 C21 C29 -77.5(4) . . . . ? S1 C14 C21 C29 108.5(3) . . . . ? La1 C14 C21 C29 -168.1(2) . . . . ? La1 O2 C22 C21 -11.7(4) . . . . ? La1 O2 C22 C23 167.89(19) . . . . ? C29 C21 C22 O2 175.1(3) . . . . ? C14 C21 C22 O2 -4.1(4) . . . . ? C29 C21 C22 C23 -4.4(4) . . . . ? C14 C21 C22 C23 176.4(3) . . . . ? O2 C22 C23 C24 -176.2(3) . . . . ? C21 C22 C23 C24 3.3(4) . . . . ? O2 C22 C23 Si2 1.0(4) . . . . ? C21 C22 C23 Si2 -179.4(2) . . . . ? C22 C23 C24 C30 0.4(4) . . . . ? Si2 C23 C24 C30 -176.8(2) . . . . ? C30 C25 C26 C27 -0.3(5) . . . . ? C25 C26 C27 C28 0.8(5) . . . . ? C26 C27 C28 C29 -0.4(5) . . . . ? C22 C21 C29 C30 1.8(4) . . . . ? C14 C21 C29 C30 -179.1(3) . . . . ? C22 C21 C29 C28 -177.4(3) . . . . ? C14 C21 C29 C28 1.7(4) . . . . ? C27 C28 C29 C30 -0.6(4) . . . . ? C27 C28 C29 C21 178.6(3) . . . . ? C26 C25 C30 C29 -0.7(5) . . . . ? C26 C25 C30 C24 179.3(3) . . . . ? C21 C29 C30 C25 -178.1(3) . . . . ? C28 C29 C30 C25 1.1(4) . . . . ? C21 C29 C30 C24 1.9(4) . . . . ? C28 C29 C30 C24 -178.9(3) . . . . ? C23 C24 C30 C25 177.0(3) . . . . ? C23 C24 C30 C29 -3.0(4) . . . . ? C24 C23 Si2 C67 98.5(3) . . . . ? C22 C23 Si2 C67 -78.7(3) . . . . ? C24 C23 Si2 C61 -131.9(2) . . . . ? C22 C23 Si2 C61 50.9(3) . . . . ? C24 C23 Si2 C73 -17.0(3) . . . . ? C22 C23 Si2 C73 165.8(2) . . . . ? C67 Si2 C61 C62 146.9(3) . . . . ? C23 Si2 C61 C62 19.8(3) . . . . ? C73 Si2 C61 C62 -97.5(3) . . . . ? C67 Si2 C61 C66 -44.0(3) . . . . ? C23 Si2 C61 C66 -171.2(3) . . . . ? C73 Si2 C61 C66 71.6(3) . . . . ? C66 C61 C62 C63 -1.8(5) . . . . ? Si2 C61 C62 C63 167.6(3) . . . . ? C61 C62 C63 C64 1.7(5) . . . . ? C62 C63 C64 C65 -0.1(5) . . . . ? C63 C64 C65 C66 -1.3(6) . . . . ? C64 C65 C66 C61 1.1(6) . . . . ? C62 C61 C66 C65 0.4(5) . . . . ? Si2 C61 C66 C65 -169.0(3) . . . . ? C61 Si2 C67 C71 -119.9(3) . . . . ? C23 Si2 C67 C71 9.0(3) . . . . ? C73 Si2 C67 C71 125.8(3) . . . . ? C61 Si2 C67 C68 65.7(3) . . . . ? C23 Si2 C67 C68 -165.4(3) . . . . ? C73 Si2 C67 C68 -48.7(3) . . . . ? C71 C67 C68 C69 1.1(5) . . . . ? Si2 C67 C68 C69 175.9(3) . . . . ? C67 C68 C69 C70 -1.7(6) . . . . ? C68 C69 C70 C72 0.2(6) . . . . ? C68 C67 C71 C72 0.9(5) . . . . ? Si2 C67 C71 C72 -173.7(3) . . . . ? C69 C70 C72 C71 1.8(6) . . . . ? C67 C71 C72 C70 -2.4(6) . . . . ? C67 Si2 C73 C78 -41.5(3) . . . . ? C61 Si2 C73 C78 -162.8(3) . . . . ? C23 Si2 C73 C78 76.4(3) . . . . ? C67 Si2 C73 C74 139.5(3) . . . . ? C61 Si2 C73 C74 18.2(3) . . . . ? C23 Si2 C73 C74 -102.6(3) . . . . ? C78 C73 C74 C75 -0.2(5) . . . . ? Si2 C73 C74 C75 178.9(2) . . . . ? C73 C74 C75 C76 -0.9(5) . . . . ? C74 C75 C76 C77 1.5(5) . . . . ? C75 C76 C77 C78 -0.9(5) . . . . ? C76 C77 C78 C73 -0.2(5) . . . . ? C74 C73 C78 C77 0.7(5) . . . . ? Si2 C73 C78 C77 -178.3(3) . . . . ? C101 C102 C103 C103 178.1(8) . . . 2_756 ? #===END data_complex10 _database_code_depnum_ccdc_archive 'CCDC 752792' #TrackingRef 'Cif_files_B920283H.cif' _audit_creation_date 2009-11-16T18:34:00-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C126 H94 La2 N2 O9 Si4, 4(C6 H6)' _chemical_formula_sum 'C150 H118 La2 N2 O9 Si4' _chemical_formula_weight 2482.64 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a b' _symmetry_space_group_name_Hall '-P 2bc 2ac' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 22.4713(9) _cell_length_b 29.6425(13) _cell_length_c 39.1800(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 26098.0(18) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7641 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.04 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.065 _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10192 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.854 _exptl_absorpt_correction_T_max 0.953 #----------------------------------------------------------------------------# # SQUEEZE RESULTS # #----------------------------------------------------------------------------# # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.266 0.250 0.395 699 -8 ' ' 2 0.234 0.250 0.895 699 -8 ' ' 3 0.500 0.208 0.036 7 0 ' ' 4 0.000 0.208 0.536 7 0 ' ' 5 0.000 0.292 0.036 7 0 ' ' 6 0.500 0.292 0.536 7 -1 ' ' 7 0.266 0.750 0.105 699 -10 ' ' 8 0.234 0.750 0.605 699 -10 ' ' 9 0.500 0.708 0.464 7 0 ' ' 10 0.000 0.708 0.964 7 0 ' ' 11 0.000 0.792 0.464 7 -1 ' ' 12 0.500 0.792 0.964 7 -1 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.1008 _diffrn_reflns_av_unetI/netI 0.0896 _diffrn_reflns_number 151425 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 29729 _reflns_number_gt 19646 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART, 2006' _computing_cell_refinement 'Bruker SMART, 2006' _computing_data_reduction 'Bruker SAINT, 2006' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0791P)^2^+115.5715P] 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_number_reflns 29729 _refine_ls_number_parameters 1024 _refine_ls_number_restraints 477 _refine_ls_R_factor_all 0.1255 _refine_ls_R_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.2032 _refine_ls_wR_factor_gt 0.1829 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.984 _refine_diff_density_min -1.388 _refine_diff_density_rms 0.123 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.174028(15) 0.066802(12) 0.147916(8) 0.02456(9) Uani 1 1 d . . . N1 N 0.2345(2) 0.04137(17) 0.20485(11) 0.0235(10) Uani 1 1 d . . . O1 O 0.20273(17) 0.13246(14) 0.17603(10) 0.0283(9) Uani 1 1 d . . . O2 O 0.11027(17) 0.02530(14) 0.18438(10) 0.0254(9) Uani 1 1 d . . . O3 O 0.0749(2) 0.11419(17) 0.15916(13) 0.0432(12) Uani 1 1 d . . . O40 O 0.1491(3) 0.1016(2) 0.08689(15) 0.080(2) Uani 1 1 d . . . Si1 Si 0.22775(8) 0.22990(6) 0.16057(5) 0.0360(4) Uani 1 1 d . . . Si4 Si 0.00105(7) -0.03040(6) 0.17065(4) 0.0249(4) Uani 1 1 d . . . C1 C 0.2962(2) 0.1113(2) 0.20040(13) 0.0262(13) Uani 1 1 d D . . C2 C 0.2594(2) 0.14208(18) 0.18371(12) 0.0263(13) Uani 1 1 d D . . C3 C 0.2829(2) 0.1843(2) 0.17213(14) 0.0284(14) Uani 1 1 d D . . C4 C 0.3425(2) 0.1937(2) 0.17738(15) 0.0315(14) Uani 1 1 d D . . H4 H 0.3576 0.2223 0.1706 0.038 Uiso 1 1 calc R . . C5 C 0.4428(3) 0.1718(3) 0.19675(19) 0.0425(17) Uani 1 1 d D . . H5 H 0.4584 0.1996 0.1886 0.051 Uiso 1 1 calc R . . C6 C 0.4799(3) 0.1414(3) 0.2127(2) 0.054(2) Uani 1 1 d D . . H6 H 0.5208 0.1485 0.2159 0.064 Uiso 1 1 calc R . . C7 C 0.4572(3) 0.1000(2) 0.22415(19) 0.0441(18) Uani 1 1 d D . . H7 H 0.4831 0.0789 0.2347 0.053 Uiso 1 1 calc R . . C8 C 0.3981(3) 0.0897(2) 0.22030(16) 0.0333(15) Uani 1 1 d D . . H8 H 0.3838 0.0614 0.2281 0.04 Uiso 1 1 calc R . . C9 C 0.3576(2) 0.1206(2) 0.20475(14) 0.0292(14) Uani 1 1 d D . . C10 C 0.3815(2) 0.1622(2) 0.19246(15) 0.0283(14) Uani 1 1 d D . . C11 C 0.2688(3) 0.0731(2) 0.22030(14) 0.0259(13) Uani 1 1 d . . . C12 C 0.2807(3) 0.0715(2) 0.25528(16) 0.0348(15) Uani 1 1 d . . . H12 H 0.3034 0.0946 0.2658 0.042 Uiso 1 1 calc R . . C13 C 0.2590(3) 0.0358(2) 0.27438(16) 0.0366(16) Uani 1 1 d . . . H13 H 0.2666 0.0342 0.2982 0.044 Uiso 1 1 calc R . . C14 C 0.2268(3) 0.0030(2) 0.25870(14) 0.0287(13) Uani 1 1 d . . . H14 H 0.2126 -0.0221 0.2715 0.034 Uiso 1 1 calc R . . C15 C 0.2143(2) 0.0061(2) 0.22372(14) 0.0238(13) Uani 1 1 d . . . C21 C 0.1751(2) -0.0294(2) 0.20838(12) 0.0216(12) Uani 1 1 d D . . C22 C 0.1202(2) -0.0164(2) 0.19389(11) 0.0233(12) Uani 1 1 d D . . C23 C 0.0748(2) -0.04949(19) 0.18759(13) 0.0234(12) Uani 1 1 d D . . C24 C 0.0851(3) -0.0941(2) 0.19672(14) 0.0266(13) Uani 1 1 d D . . H24 H 0.0539 -0.1154 0.1942 0.032 Uiso 1 1 calc R . . C25 C 0.1514(3) -0.1545(2) 0.21732(15) 0.0323(14) Uani 1 1 d D . . H25 H 0.1201 -0.1757 0.2144 0.039 Uiso 1 1 calc R . . C26 C 0.2062(3) -0.1690(2) 0.22885(17) 0.0382(16) Uani 1 1 d D . . H26 H 0.2128 -0.1999 0.234 0.046 Uiso 1 1 calc R . . C27 C 0.2523(3) -0.1372(2) 0.23282(15) 0.0355(16) Uani 1 1 d D . . H27 H 0.2905 -0.1471 0.24 0.043 Uiso 1 1 calc R . . C28 C 0.2433(3) -0.0921(2) 0.22661(14) 0.0286(14) Uani 1 1 d D . . H28 H 0.2752 -0.0715 0.2296 0.034 Uiso 1 1 calc R . . C29 C 0.1867(2) -0.0757(2) 0.21571(14) 0.0251(13) Uani 1 1 d D . . C30 C 0.1412(3) -0.1087(2) 0.20981(14) 0.0277(13) Uani 1 1 d D . . C31 C 0.0613(4) 0.1211(3) 0.1956(2) 0.065(3) Uani 1 1 d . . . H31A H 0.0927 0.1395 0.2065 0.078 Uiso 1 1 calc R . . H31B H 0.059 0.0917 0.2075 0.078 Uiso 1 1 calc R . . C32 C 0.0030(4) 0.1448(3) 0.1973(3) 0.071(3) Uani 1 1 d . . . H32A H 0.0013 0.1655 0.2172 0.085 Uiso 1 1 calc R . . H32B H -0.0304 0.1231 0.1988 0.085 Uiso 1 1 calc R . . C33 C 0.0017(4) 0.1705(4) 0.1640(3) 0.081(3) Uani 1 1 d . . . H33A H -0.0385 0.1692 0.1538 0.097 Uiso 1 1 calc R . . H33B H 0.0122 0.2026 0.1679 0.097 Uiso 1 1 calc R . . C34 C 0.0453(5) 0.1492(3) 0.1413(2) 0.082(3) Uani 1 1 d . . . H34A H 0.025 0.1367 0.121 0.099 Uiso 1 1 calc R . . H34B H 0.0746 0.1719 0.1335 0.099 Uiso 1 1 calc R . . C41 C 0.1724(4) 0.2344(3) 0.1979(3) 0.0718(12) Uani 1 1 d D . . C42 C 0.1819(4) 0.2096(3) 0.2281(2) 0.0718(12) Uani 1 1 d D . . H42 H 0.2165 0.1912 0.2286 0.086 Uiso 1 1 calc R . . C43 C 0.1457(4) 0.2090(3) 0.2579(3) 0.0718(12) Uani 1 1 d D . . H43 H 0.1553 0.1925 0.2779 0.086 Uiso 1 1 calc R . . C44 C 0.0955(4) 0.2349(3) 0.2545(3) 0.0718(12) Uani 1 1 d D . . H44 H 0.0673 0.2334 0.2726 0.086 Uiso 1 1 calc R . . C45 C 0.0817(4) 0.2632(3) 0.2274(2) 0.0718(12) Uani 1 1 d D . . H45 H 0.0471 0.2816 0.2274 0.086 Uiso 1 1 calc R . . C46 C 0.1228(4) 0.2628(3) 0.1992(3) 0.0718(12) Uani 1 1 d D . . H46 H 0.1159 0.2828 0.1807 0.086 Uiso 1 1 calc R . . C47 C 0.2683(3) 0.2853(3) 0.15654(19) 0.0523(8) Uani 1 1 d D . . C48 C 0.2936(3) 0.3059(2) 0.1847(2) 0.0523(8) Uani 1 1 d D . . H48 H 0.2895 0.2922 0.2065 0.063 Uiso 1 1 calc R . . C49 C 0.3249(3) 0.3463(2) 0.1818(2) 0.0523(8) Uani 1 1 d D . . H49 H 0.3412 0.3598 0.2017 0.063 Uiso 1 1 calc R . . C50 C 0.3327(4) 0.3668(3) 0.15055(18) 0.0523(8) Uani 1 1 d D . . H50 H 0.3552 0.3939 0.1486 0.063 Uiso 1 1 calc R . . C51 C 0.3070(3) 0.3471(3) 0.1223(2) 0.0523(8) Uani 1 1 d D . . H51 H 0.3103 0.3613 0.1006 0.063 Uiso 1 1 calc R . . C52 C 0.2765(4) 0.3067(2) 0.1254(2) 0.0523(8) Uani 1 1 d D . . H52 H 0.2605 0.2931 0.1054 0.063 Uiso 1 1 calc R . . C53 C 0.1901(3) 0.2198(3) 0.1179(2) 0.0542(9) Uani 1 1 d D . . C54 C 0.1337(3) 0.2358(2) 0.1089(2) 0.0542(9) Uani 1 1 d D . . H54 H 0.1107 0.251 0.1257 0.065 Uiso 1 1 calc R . . C55 C 0.1100(3) 0.2305(3) 0.07666(19) 0.0542(9) Uani 1 1 d D . . H55 H 0.0712 0.2415 0.0717 0.065 Uiso 1 1 calc R . . C56 C 0.1427(3) 0.2093(3) 0.0520(2) 0.0542(9) Uani 1 1 d D . . H56 H 0.1262 0.2049 0.0299 0.065 Uiso 1 1 calc R . . C57 C 0.1998(3) 0.1942(3) 0.0591(2) 0.0542(9) Uani 1 1 d D . . H57 H 0.2231 0.1802 0.0419 0.065 Uiso 1 1 calc R . . C58 C 0.2225(4) 0.1997(3) 0.09174(19) 0.0542(9) Uani 1 1 d D . . H58 H 0.2617 0.1894 0.0964 0.065 Uiso 1 1 calc R . . C61 C -0.0445(5) -0.0810(4) 0.1592(2) 0.0993(18) Uani 1 1 d D . . C62 C -0.0416(5) -0.1000(3) 0.1265(2) 0.0993(18) Uani 1 1 d D . . H62 H -0.0195 -0.0851 0.1092 0.119 Uiso 1 1 calc R . . C63 C -0.0706(5) -0.1404(3) 0.1191(2) 0.0993(18) Uani 1 1 d D . . H63 H -0.0662 -0.1537 0.0972 0.119 Uiso 1 1 calc R . . C64 C -0.1062(5) -0.1614(4) 0.1439(2) 0.0993(18) Uani 1 1 d D . . H64 H -0.1278 -0.1881 0.1386 0.119 Uiso 1 1 calc R . . C65 C -0.1093(6) -0.1426(4) 0.1763(2) 0.0993(18) Uani 1 1 d D . . H65 H -0.1332 -0.1564 0.1933 0.119 Uiso 1 1 calc R . . C66 C -0.0777(5) -0.1040(4) 0.1837(2) 0.0993(18) Uani 1 1 d D . . H66 H -0.0786 -0.0926 0.2064 0.119 Uiso 1 1 calc R . . C67 C -0.0403(3) 0.0029(2) 0.20357(16) 0.0362(6) Uani 1 1 d D . . C68 C -0.0993(3) 0.0165(2) 0.19813(16) 0.0362(6) Uani 1 1 d D . . H68 H -0.1195 0.0063 0.1783 0.043 Uiso 1 1 calc R . . C69 C -0.1293(3) 0.0447(2) 0.22096(15) 0.0362(6) Uani 1 1 d D . . H69 H -0.1689 0.054 0.2163 0.043 Uiso 1 1 calc R . . C70 C -0.1009(3) 0.0588(2) 0.25026(16) 0.0362(6) Uani 1 1 d D . . H70 H -0.1209 0.0782 0.2657 0.043 Uiso 1 1 calc R . . C71 C -0.0430(3) 0.0447(2) 0.25732(16) 0.0362(6) Uani 1 1 d D . . H71 H -0.0242 0.0532 0.2781 0.043 Uiso 1 1 calc R . . C72 C -0.0128(3) 0.0180(2) 0.23360(15) 0.0362(6) Uani 1 1 d D . . H72 H 0.0274 0.0099 0.2379 0.043 Uiso 1 1 calc R . . C73 C 0.0103(3) 0.0034(2) 0.13065(16) 0.0356(6) Uani 1 1 d D . . C74 C -0.0306(3) 0.0363(2) 0.12097(15) 0.0356(6) Uani 1 1 d D . . H74 H -0.0638 0.0424 0.1353 0.043 Uiso 1 1 calc R . . C75 C -0.0240(3) 0.0605(2) 0.09083(15) 0.0356(6) Uani 1 1 d D . . H75 H -0.0521 0.0832 0.085 0.043 Uiso 1 1 calc R . . C76 C 0.0235(3) 0.0516(2) 0.06918(16) 0.0356(6) Uani 1 1 d D . . H76 H 0.0276 0.0677 0.0483 0.043 Uiso 1 1 calc R . . C77 C 0.0645(3) 0.0194(2) 0.07815(15) 0.0356(6) Uani 1 1 d D . . H77 H 0.097 0.0129 0.0635 0.043 Uiso 1 1 calc R . . C78 C 0.0582(3) -0.0036(2) 0.10874(15) 0.0356(6) Uani 1 1 d D . . H78 H 0.0878 -0.025 0.115 0.043 Uiso 1 1 calc R . . La2 La 0.298128(15) 0.018576(14) 0.082789(8) 0.02813(10) Uani 1 1 d . . . N1B N 0.2914(2) 0.08400(17) 0.03477(12) 0.0254(11) Uani 1 1 d . . . O1B O 0.39525(17) 0.04320(15) 0.06923(10) 0.0280(9) Uani 1 1 d . . . O2B O 0.26318(17) -0.01453(15) 0.03206(10) 0.0291(10) Uani 1 1 d . . . O40B O 0.3698(3) -0.0526(2) 0.07047(15) 0.0690(17) Uani 1 1 d . . . Si1B Si 0.49870(7) 0.04404(7) 0.11682(4) 0.0281(4) Uani 1 1 d . . . Si2B Si 0.18763(7) -0.09523(6) 0.01673(4) 0.0252(4) Uani 1 1 d . . . C1B C 0.3785(3) 0.1227(2) 0.06147(14) 0.0321(14) Uani 1 1 d D . . C2B C 0.4089(2) 0.0862(2) 0.07616(12) 0.0248(13) Uani 1 1 d D . . C3B C 0.4546(2) 0.0937(2) 0.10140(13) 0.0279(14) Uani 1 1 d D . . C4B C 0.4672(3) 0.1379(2) 0.11067(14) 0.0316(15) Uani 1 1 d D . . H4B H 0.4976 0.1432 0.127 0.038 Uiso 1 1 calc R . . C5B C 0.4497(3) 0.2195(2) 0.10786(18) 0.0434(18) Uani 1 1 d D . . H5B H 0.4797 0.224 0.1246 0.052 Uiso 1 1 calc R . . C6B C 0.4197(4) 0.2563(3) 0.09473(19) 0.052(2) Uani 1 1 d D . . H6B H 0.4285 0.2859 0.1025 0.062 Uiso 1 1 calc R . . C7B C 0.3758(4) 0.2491(3) 0.06965(19) 0.054(2) Uani 1 1 d D . . H7B H 0.3551 0.2742 0.0604 0.064 Uiso 1 1 calc R . . C8B C 0.3624(3) 0.2063(2) 0.05822(18) 0.0446(18) Uani 1 1 d D . . H8B H 0.3328 0.2026 0.0411 0.054 Uiso 1 1 calc R . . C9B C 0.3917(3) 0.1678(2) 0.07142(15) 0.0308(14) Uani 1 1 d D . . C10B C 0.4366(3) 0.1754(2) 0.09677(15) 0.0328(15) Uani 1 1 d D . . C11B C 0.3380(3) 0.1135(2) 0.03167(15) 0.0294(14) Uani 1 1 d . . . C12B C 0.3490(3) 0.1355(2) 0.00086(16) 0.0349(15) Uani 1 1 d . . . H12B H 0.3817 0.1557 -0.001 0.042 Uiso 1 1 calc R . . C13B C 0.3128(3) 0.1282(3) -0.02691(16) 0.0365(16) Uani 1 1 d . . . H13B H 0.3204 0.143 -0.048 0.044 Uiso 1 1 calc R . . C14B C 0.2653(3) 0.0991(2) -0.02359(15) 0.0326(15) Uani 1 1 d . . . H14B H 0.2396 0.0938 -0.0424 0.039 Uiso 1 1 calc R . . C15B C 0.2550(2) 0.0773(2) 0.00774(14) 0.0247(13) Uani 1 1 d . . . C21B C 0.2030(2) 0.0452(2) 0.00983(13) 0.0262(13) Uani 1 1 d D . . C22B C 0.2133(2) -0.00060(19) 0.01727(11) 0.0247(13) Uani 1 1 d D . . C23B C 0.1685(2) -0.0336(2) 0.01066(13) 0.0245(12) Uani 1 1 d D . . C24B C 0.1145(2) -0.0198(2) -0.00366(14) 0.0247(12) Uani 1 1 d D . . H24B H 0.0853 -0.0418 -0.0092 0.03 Uiso 1 1 calc R . . C25B C 0.0462(2) 0.0397(2) -0.02341(14) 0.0277(13) Uani 1 1 d D . . H25B H 0.0169 0.0175 -0.028 0.033 Uiso 1 1 calc R . . C26B C 0.0339(3) 0.0846(2) -0.02962(15) 0.0311(14) Uani 1 1 d D . . H26B H -0.0033 0.0932 -0.0391 0.037 Uiso 1 1 calc R . . C27B C 0.0773(3) 0.1177(2) -0.02175(15) 0.0309(14) Uani 1 1 d D . . H27B H 0.0683 0.1487 -0.0251 0.037 Uiso 1 1 calc R . . C28B C 0.1321(3) 0.1054(2) -0.00939(14) 0.0279(13) Uani 1 1 d D . . H28B H 0.161 0.128 -0.0048 0.033 Uiso 1 1 calc R . . C29B C 0.1462(2) 0.0590(2) -0.00327(14) 0.0277(14) Uani 1 1 d D . . C30B C 0.1025(2) 0.02668(19) -0.01014(13) 0.0230(12) Uani 1 1 d D . . C41B C 0.5429(3) 0.0184(3) 0.08123(15) 0.0403(7) Uani 1 1 d D . . C42B C 0.5307(3) 0.0259(2) 0.04661(14) 0.0403(7) Uani 1 1 d D . . H42B H 0.4966 0.043 0.0405 0.048 Uiso 1 1 calc R . . C43B C 0.5673(3) 0.0089(2) 0.02088(16) 0.0403(7) Uani 1 1 d D . . H43B H 0.5578 0.0145 -0.0024 0.048 Uiso 1 1 calc R . . C44B C 0.6174(3) -0.0162(3) 0.02908(15) 0.0403(7) Uani 1 1 d D . . H44B H 0.6423 -0.0279 0.0116 0.048 Uiso 1 1 calc R . . C45B C 0.6306(3) -0.0239(3) 0.06313(15) 0.0403(7) Uani 1 1 d D . . H45B H 0.6647 -0.0411 0.0691 0.048 Uiso 1 1 calc R . . C46B C 0.5938(3) -0.0065(3) 0.08863(16) 0.0403(7) Uani 1 1 d D . . H46B H 0.6039 -0.0118 0.1118 0.048 Uiso 1 1 calc R . . C47B C 0.5556(3) 0.0624(2) 0.14883(14) 0.0342(6) Uani 1 1 d D . . C48B C 0.5998(2) 0.0938(2) 0.13996(15) 0.0342(6) Uani 1 1 d D . . H48B H 0.6003 0.105 0.1173 0.041 Uiso 1 1 calc R . . C49B C 0.6426(3) 0.1093(2) 0.16244(14) 0.0342(6) Uani 1 1 d D . . H49B H 0.6714 0.1308 0.1553 0.041 Uiso 1 1 calc R . . C50B C 0.6426(3) 0.0928(2) 0.19585(14) 0.0342(6) Uani 1 1 d D . . H50B H 0.6713 0.1032 0.2119 0.041 Uiso 1 1 calc R . . C51B C 0.6009(3) 0.0613(2) 0.20530(15) 0.0342(6) Uani 1 1 d D . . H51B H 0.6012 0.0496 0.2279 0.041 Uiso 1 1 calc R . . C52B C 0.5578(3) 0.0461(2) 0.18218(14) 0.0342(6) Uani 1 1 d D . . H52B H 0.5295 0.0242 0.1893 0.041 Uiso 1 1 calc R . . C53B C 0.4480(3) 0.0008(2) 0.13679(15) 0.0357(6) Uani 1 1 d D . . C54B C 0.4631(3) -0.0446(2) 0.13844(15) 0.0357(6) Uani 1 1 d D . . H54B H 0.5013 -0.0537 0.1308 0.043 Uiso 1 1 calc R . . C55B C 0.4244(3) -0.0772(2) 0.15086(15) 0.0357(6) Uani 1 1 d D . . H55B H 0.4366 -0.1079 0.1517 0.043 Uiso 1 1 calc R . . C56B C 0.3681(3) -0.0651(2) 0.16201(16) 0.0357(6) Uani 1 1 d D . . H56B H 0.3411 -0.0874 0.17 0.043 Uiso 1 1 calc R . . C57B C 0.3515(3) -0.0199(2) 0.16129(15) 0.0357(6) Uani 1 1 d D . . H57B H 0.3131 -0.0111 0.169 0.043 Uiso 1 1 calc R . . C58B C 0.3915(3) 0.0127(2) 0.14919(15) 0.0357(6) Uani 1 1 d D . . H58B H 0.3801 0.0435 0.1494 0.043 Uiso 1 1 calc R . . C61B C 0.2077(3) -0.1084(2) 0.06210(16) 0.0423(7) Uani 1 1 d D . . C62B C 0.2606(3) -0.1301(2) 0.07131(16) 0.0423(7) Uani 1 1 d D . . H62B H 0.2889 -0.1375 0.0542 0.051 Uiso 1 1 calc R . . C63B C 0.2725(3) -0.1411(2) 0.10518(15) 0.0423(7) Uani 1 1 d D . . H63B H 0.3086 -0.1561 0.1107 0.051 Uiso 1 1 calc R . . C64B C 0.2327(3) -0.1307(3) 0.13093(17) 0.0423(7) Uani 1 1 d D . . H64B H 0.2419 -0.1372 0.1541 0.051 Uiso 1 1 calc R . . C65B C 0.1793(3) -0.1106(3) 0.12225(16) 0.0423(7) Uani 1 1 d D . . H65B H 0.1507 -0.1043 0.1394 0.051 Uiso 1 1 calc R . . C66B C 0.1674(3) -0.0998(3) 0.08847(15) 0.0423(7) Uani 1 1 d D . . H66B H 0.1305 -0.0859 0.0831 0.051 Uiso 1 1 calc R . . C67B C 0.1213(3) -0.1325(2) 0.00657(16) 0.0387(7) Uani 1 1 d D . . C68B C 0.0998(3) -0.1649(2) 0.02922(17) 0.0387(7) Uani 1 1 d D . . H68B H 0.1164 -0.1667 0.0515 0.046 Uiso 1 1 calc R . . C69B C 0.0544(3) -0.1948(2) 0.02003(17) 0.0387(7) Uani 1 1 d D . . H69B H 0.0409 -0.2167 0.0359 0.046 Uiso 1 1 calc R . . C70B C 0.0289(3) -0.1925(2) -0.01216(16) 0.0387(7) Uani 1 1 d D . . H70B H -0.0019 -0.2128 -0.0185 0.046 Uiso 1 1 calc R . . C71B C 0.0490(3) -0.1603(2) -0.03485(18) 0.0387(7) Uani 1 1 d D . . H71B H 0.0314 -0.1581 -0.0568 0.046 Uiso 1 1 calc R . . C72B C 0.0949(3) -0.1310(2) -0.02573(17) 0.0387(7) Uani 1 1 d D . . H72B H 0.1086 -0.1095 -0.0419 0.046 Uiso 1 1 calc R . . C73B C 0.2477(3) -0.1146(2) -0.01315(16) 0.0382(7) Uani 1 1 d D . . C74B C 0.2509(3) -0.1602(2) -0.02185(15) 0.0382(7) Uani 1 1 d D . . H74B H 0.2223 -0.1804 -0.0127 0.046 Uiso 1 1 calc R . . C75B C 0.2946(3) -0.1768(2) -0.04343(16) 0.0382(7) Uani 1 1 d D . . H75B H 0.2957 -0.208 -0.049 0.046 Uiso 1 1 calc R . . C76B C 0.3365(3) -0.1477(2) -0.05670(17) 0.0382(7) Uani 1 1 d D . . H76B H 0.3671 -0.1589 -0.0712 0.046 Uiso 1 1 calc R . . C77B C 0.3341(3) -0.1022(2) -0.04894(16) 0.0382(7) Uani 1 1 d D . . H77B H 0.3624 -0.0821 -0.0585 0.046 Uiso 1 1 calc R . . C78B C 0.2902(3) -0.0860(2) -0.02713(16) 0.0382(7) Uani 1 1 d D . . H78B H 0.2893 -0.0548 -0.0217 0.046 Uiso 1 1 calc R . . O51 O 0.27064(18) 0.08021(16) 0.11853(11) 0.0346(10) Uani 1 1 d . . . O52 O 0.21177(19) 0.00046(16) 0.11751(12) 0.0372(11) Uani 1 1 d . . . C501 C 0.4415(7) 0.1525(6) 0.8246(4) 0.146(3) Uani 1 1 d D . . H501 H 0.4665 0.1784 0.8241 0.175 Uiso 1 1 calc R . . C502 C 0.4076(6) 0.1425(6) 0.8533(4) 0.146(3) Uani 1 1 d D . . H502 H 0.409 0.1614 0.8729 0.175 Uiso 1 1 calc R . . C503 C 0.3723(7) 0.1054(5) 0.8527(4) 0.146(3) Uani 1 1 d D . . H503 H 0.3481 0.0982 0.8718 0.175 Uiso 1 1 calc R . . C504 C 0.3719(8) 0.0782(6) 0.8244(4) 0.146(3) Uani 1 1 d D . . H504 H 0.3509 0.0504 0.8258 0.175 Uiso 1 1 calc R . . C505 C 0.3990(7) 0.0880(6) 0.7947(4) 0.146(3) Uani 1 1 d D . . H505 H 0.392 0.0717 0.7742 0.175 Uiso 1 1 calc R . . C506 C 0.4384(8) 0.1242(5) 0.7968(4) 0.146(3) Uani 1 1 d D . . H506 H 0.4643 0.1297 0.7781 0.175 Uiso 1 1 calc R . . C511 C 0.2397(7) 0.0034(5) 0.3661(3) 0.130(3) Uani 1 1 d D . . H511 H 0.2096 -0.0039 0.3501 0.156 Uiso 1 1 calc R . . C512 C 0.2587(6) -0.0269(6) 0.3881(3) 0.130(3) Uani 1 1 d D . . H512 H 0.2406 -0.0558 0.3888 0.156 Uiso 1 1 calc R . . C513 C 0.3038(6) -0.0170(6) 0.4097(3) 0.130(3) Uani 1 1 d D . . H513 H 0.3165 -0.0381 0.4265 0.156 Uiso 1 1 calc R . . C514 C 0.3299(7) 0.0234(5) 0.4068(3) 0.130(3) Uani 1 1 d D . . H514 H 0.364 0.0303 0.4201 0.156 Uiso 1 1 calc R . . C515 C 0.3081(6) 0.0541(6) 0.3850(3) 0.130(3) Uani 1 1 d D . . H515 H 0.3254 0.0832 0.383 0.156 Uiso 1 1 calc R . . C516 C 0.2624(6) 0.0425(6) 0.3668(3) 0.130(3) Uani 1 1 d D . . H516 H 0.2445 0.065 0.3529 0.156 Uiso 1 1 calc R . . C521 C 0.1910(6) 0.2434(4) 0.7967(3) 0.0965(16) Uani 1 1 d D . . H521 H 0.225 0.2246 0.7994 0.116 Uiso 1 1 calc R . . C522 C 0.1751(5) 0.2724(4) 0.8224(3) 0.0965(16) Uani 1 1 d D . . H522 H 0.1977 0.2734 0.8429 0.116 Uiso 1 1 calc R . . C523 C 0.1265(5) 0.2999(4) 0.8184(3) 0.0965(16) Uani 1 1 d D . . H523 H 0.1152 0.3192 0.8366 0.116 Uiso 1 1 calc R . . C524 C 0.0936(6) 0.3002(4) 0.7885(3) 0.0965(16) Uani 1 1 d D . . H524 H 0.0617 0.3209 0.7853 0.116 Uiso 1 1 calc R . . C525 C 0.1089(5) 0.2691(4) 0.7633(3) 0.0965(16) Uani 1 1 d D . . H525 H 0.0852 0.267 0.7433 0.116 Uiso 1 1 calc R . . C526 C 0.1583(5) 0.2411(4) 0.7668(3) 0.0965(16) Uani 1 1 d D . . H526 H 0.1692 0.2209 0.7491 0.116 Uiso 1 1 calc R . . C531 C 0.4580(5) 0.8616(5) 0.0104(4) 0.129(2) Uani 1 1 d D . . H531 H 0.454 0.867 -0.0134 0.155 Uiso 1 1 calc R . . C532 C 0.4205(6) 0.8306(5) 0.0259(3) 0.129(2) Uani 1 1 d D . . H532 H 0.3897 0.8167 0.0131 0.155 Uiso 1 1 calc R . . C533 C 0.4278(6) 0.8200(5) 0.0598(4) 0.129(2) Uani 1 1 d D . . H533 H 0.4027 0.7987 0.0709 0.155 Uiso 1 1 calc R . . C534 C 0.4736(6) 0.8418(5) 0.0772(4) 0.129(2) Uani 1 1 d D . . H534 H 0.4803 0.8349 0.1006 0.155 Uiso 1 1 calc R . . C535 C 0.5099(6) 0.8734(5) 0.0611(4) 0.129(2) Uani 1 1 d D . . H535 H 0.5414 0.8873 0.0733 0.155 Uiso 1 1 calc R . . C536 C 0.4998(6) 0.8842(6) 0.0280(4) 0.129(2) Uani 1 1 d D . . H536 H 0.522 0.9075 0.0173 0.155 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 0.02076(16) 0.0339(2) 0.01899(16) 0.00346(15) -0.00102(13) 0.00193(15) N1 0.021(2) 0.030(3) 0.020(2) -0.002(2) -0.0036(19) 0.007(2) O1 0.020(2) 0.034(2) 0.030(2) 0.0015(19) 0.0013(17) 0.0040(18) O2 0.024(2) 0.029(2) 0.023(2) 0.0018(18) 0.0007(16) 0.0055(17) O3 0.036(3) 0.046(3) 0.047(3) 0.008(2) 0.002(2) 0.015(2) O40 0.120(6) 0.074(4) 0.044(3) 0.019(3) -0.028(4) -0.028(4) Si1 0.0270(9) 0.0281(10) 0.0529(12) 0.0006(9) -0.0116(8) -0.0028(8) Si4 0.0202(8) 0.0318(10) 0.0227(8) 0.0049(7) -0.0005(6) 0.0013(7) C1 0.028(3) 0.028(3) 0.023(3) -0.003(2) 0.001(2) 0.008(3) C2 0.023(3) 0.027(3) 0.030(3) -0.007(3) 0.006(2) -0.003(2) C3 0.025(3) 0.036(4) 0.023(3) -0.002(3) -0.003(2) 0.004(3) C4 0.030(3) 0.037(4) 0.028(3) -0.003(3) 0.001(3) -0.003(3) C5 0.028(4) 0.047(5) 0.052(4) -0.008(4) -0.007(3) 0.001(3) C6 0.030(4) 0.057(5) 0.073(6) -0.014(4) -0.017(4) 0.007(4) C7 0.034(4) 0.045(5) 0.053(5) -0.007(4) -0.019(3) 0.012(3) C8 0.028(3) 0.032(4) 0.040(4) -0.011(3) -0.004(3) 0.003(3) C9 0.024(3) 0.043(4) 0.021(3) -0.008(3) -0.003(2) 0.005(3) C10 0.022(3) 0.035(4) 0.028(3) -0.008(3) -0.004(2) 0.005(3) C11 0.028(3) 0.030(3) 0.020(3) 0.002(2) -0.002(2) 0.004(3) C12 0.039(4) 0.036(4) 0.029(3) -0.009(3) -0.006(3) -0.002(3) C13 0.045(4) 0.040(4) 0.025(3) 0.001(3) -0.004(3) 0.007(3) C14 0.032(3) 0.035(4) 0.019(3) 0.006(3) -0.003(2) -0.002(3) C15 0.021(3) 0.032(3) 0.019(3) 0.002(2) -0.004(2) 0.008(2) C21 0.019(3) 0.030(3) 0.016(2) 0.001(2) 0.005(2) 0.007(2) C22 0.025(3) 0.030(3) 0.016(3) 0.003(2) 0.005(2) 0.003(2) C23 0.023(3) 0.035(3) 0.013(2) 0.002(2) 0.005(2) 0.007(2) C24 0.028(3) 0.035(4) 0.017(3) 0.008(3) -0.002(2) -0.001(3) C25 0.037(4) 0.030(4) 0.030(3) 0.003(3) -0.003(3) 0.005(3) C26 0.048(4) 0.032(4) 0.034(4) 0.004(3) -0.002(3) 0.012(3) C27 0.036(4) 0.045(4) 0.025(3) 0.010(3) 0.002(3) 0.017(3) C28 0.029(3) 0.036(4) 0.021(3) 0.005(3) 0.002(2) 0.006(3) C29 0.024(3) 0.036(4) 0.015(3) 0.001(2) 0.003(2) 0.006(2) C30 0.033(3) 0.033(4) 0.017(3) 0.003(3) 0.005(2) 0.010(3) C31 0.057(5) 0.076(7) 0.062(6) 0.014(5) 0.022(4) 0.025(5) C32 0.051(5) 0.067(6) 0.095(7) 0.009(6) 0.023(5) 0.023(5) C33 0.066(6) 0.101(8) 0.075(7) 0.015(6) 0.004(5) 0.039(6) C34 0.127(10) 0.064(6) 0.056(6) 0.017(5) -0.008(6) 0.040(6) C41 0.053(2) 0.071(3) 0.092(3) -0.024(2) 0.008(2) 0.002(2) C42 0.053(2) 0.071(3) 0.092(3) -0.024(2) 0.008(2) 0.002(2) C43 0.053(2) 0.071(3) 0.092(3) -0.024(2) 0.008(2) 0.002(2) C44 0.053(2) 0.071(3) 0.092(3) -0.024(2) 0.008(2) 0.002(2) C45 0.053(2) 0.071(3) 0.092(3) -0.024(2) 0.008(2) 0.002(2) C46 0.053(2) 0.071(3) 0.092(3) -0.024(2) 0.008(2) 0.002(2) C47 0.056(2) 0.0433(19) 0.058(2) -0.0043(16) -0.0022(16) -0.0154(15) C48 0.056(2) 0.0433(19) 0.058(2) -0.0043(16) -0.0022(16) -0.0154(15) C49 0.056(2) 0.0433(19) 0.058(2) -0.0043(16) -0.0022(16) -0.0154(15) C50 0.056(2) 0.0433(19) 0.058(2) -0.0043(16) -0.0022(16) -0.0154(15) C51 0.056(2) 0.0433(19) 0.058(2) -0.0043(16) -0.0022(16) -0.0154(15) C52 0.056(2) 0.0433(19) 0.058(2) -0.0043(16) -0.0022(16) -0.0154(15) C53 0.0461(19) 0.048(2) 0.068(2) 0.0093(17) -0.0273(16) -0.0079(15) C54 0.0461(19) 0.048(2) 0.068(2) 0.0093(17) -0.0273(16) -0.0079(15) C55 0.0461(19) 0.048(2) 0.068(2) 0.0093(17) -0.0273(16) -0.0079(15) C56 0.0461(19) 0.048(2) 0.068(2) 0.0093(17) -0.0273(16) -0.0079(15) C57 0.0461(19) 0.048(2) 0.068(2) 0.0093(17) -0.0273(16) -0.0079(15) C58 0.0461(19) 0.048(2) 0.068(2) 0.0093(17) -0.0273(16) -0.0079(15) C61 0.152(5) 0.098(4) 0.048(2) 0.008(2) -0.005(3) -0.082(3) C62 0.152(5) 0.098(4) 0.048(2) 0.008(2) -0.005(3) -0.082(3) C63 0.152(5) 0.098(4) 0.048(2) 0.008(2) -0.005(3) -0.082(3) C64 0.152(5) 0.098(4) 0.048(2) 0.008(2) -0.005(3) -0.082(3) C65 0.152(5) 0.098(4) 0.048(2) 0.008(2) -0.005(3) -0.082(3) C66 0.152(5) 0.098(4) 0.048(2) 0.008(2) -0.005(3) -0.082(3) C67 0.0278(13) 0.0490(18) 0.0319(14) 0.0079(13) 0.0079(11) 0.0069(12) C68 0.0278(13) 0.0490(18) 0.0319(14) 0.0079(13) 0.0079(11) 0.0069(12) C69 0.0278(13) 0.0490(18) 0.0319(14) 0.0079(13) 0.0079(11) 0.0069(12) C70 0.0278(13) 0.0490(18) 0.0319(14) 0.0079(13) 0.0079(11) 0.0069(12) C71 0.0278(13) 0.0490(18) 0.0319(14) 0.0079(13) 0.0079(11) 0.0069(12) C72 0.0278(13) 0.0490(18) 0.0319(14) 0.0079(13) 0.0079(11) 0.0069(12) C73 0.0342(14) 0.0450(17) 0.0276(13) 0.0090(12) 0.0020(11) 0.0086(12) C74 0.0342(14) 0.0450(17) 0.0276(13) 0.0090(12) 0.0020(11) 0.0086(12) C75 0.0342(14) 0.0450(17) 0.0276(13) 0.0090(12) 0.0020(11) 0.0086(12) C76 0.0342(14) 0.0450(17) 0.0276(13) 0.0090(12) 0.0020(11) 0.0086(12) C77 0.0342(14) 0.0450(17) 0.0276(13) 0.0090(12) 0.0020(11) 0.0086(12) C78 0.0342(14) 0.0450(17) 0.0276(13) 0.0090(12) 0.0020(11) 0.0086(12) La2 0.02122(17) 0.0478(2) 0.01532(15) -0.00245(15) -0.00296(13) 0.00380(16) N1B 0.024(3) 0.032(3) 0.020(2) -0.004(2) -0.003(2) 0.008(2) O1B 0.025(2) 0.041(3) 0.0183(19) -0.0049(19) -0.0065(16) 0.0058(19) O2B 0.023(2) 0.040(3) 0.025(2) 0.0013(19) -0.0036(17) 0.0111(19) O40B 0.074(4) 0.075(4) 0.057(4) -0.009(3) -0.011(3) 0.022(3) Si1B 0.0195(8) 0.0490(11) 0.0157(7) -0.0059(7) -0.0014(6) 0.0027(7) Si2B 0.0248(8) 0.0320(10) 0.0188(7) -0.0020(7) -0.0045(6) 0.0070(7) C1B 0.031(3) 0.040(4) 0.026(3) 0.001(3) 0.001(3) -0.002(3) C2B 0.017(3) 0.039(4) 0.018(3) -0.004(3) 0.001(2) -0.001(2) C3B 0.021(3) 0.047(4) 0.015(3) -0.001(3) 0.003(2) -0.001(3) C4B 0.019(3) 0.058(5) 0.017(3) -0.002(3) 0.000(2) -0.006(3) C5B 0.046(4) 0.049(5) 0.035(4) 0.003(3) -0.005(3) -0.013(4) C6B 0.069(5) 0.038(5) 0.047(4) 0.008(4) -0.015(4) -0.020(4) C7B 0.062(5) 0.046(5) 0.052(5) 0.009(4) -0.016(4) -0.008(4) C8B 0.047(4) 0.052(5) 0.035(4) 0.005(3) -0.014(3) -0.014(4) C9B 0.029(3) 0.040(4) 0.023(3) 0.005(3) -0.003(2) -0.010(3) C10B 0.036(4) 0.040(4) 0.023(3) 0.000(3) 0.001(3) -0.009(3) C11B 0.023(3) 0.041(4) 0.024(3) 0.001(3) -0.006(2) -0.002(3) C12B 0.027(3) 0.045(4) 0.033(3) 0.003(3) -0.002(3) -0.002(3) C13B 0.034(4) 0.055(5) 0.021(3) 0.008(3) 0.001(3) 0.000(3) C14B 0.031(3) 0.047(4) 0.019(3) 0.000(3) -0.007(3) 0.007(3) C15B 0.021(3) 0.035(4) 0.018(3) -0.005(2) -0.003(2) 0.008(2) C21B 0.017(3) 0.043(4) 0.019(3) -0.006(3) -0.006(2) 0.007(3) C22B 0.024(3) 0.038(4) 0.012(2) -0.004(2) -0.002(2) 0.010(3) C23B 0.022(3) 0.032(3) 0.019(3) -0.002(2) -0.001(2) 0.010(2) C24B 0.020(3) 0.031(3) 0.022(3) -0.008(3) -0.001(2) -0.001(2) C25B 0.022(3) 0.037(4) 0.025(3) 0.000(3) -0.003(2) 0.004(3) C26B 0.022(3) 0.042(4) 0.028(3) 0.002(3) -0.007(2) 0.008(3) C27B 0.035(3) 0.026(3) 0.031(3) 0.001(3) -0.001(3) 0.008(3) C28B 0.025(3) 0.037(4) 0.022(3) -0.006(3) -0.005(2) 0.006(3) C29B 0.025(3) 0.041(4) 0.017(3) -0.004(3) -0.003(2) 0.007(3) C30B 0.022(3) 0.032(3) 0.015(3) 0.000(2) -0.003(2) 0.009(2) C41B 0.0291(14) 0.068(2) 0.0239(13) -0.0124(14) -0.0013(11) 0.0070(13) C42B 0.0291(14) 0.068(2) 0.0239(13) -0.0124(14) -0.0013(11) 0.0070(13) C43B 0.0291(14) 0.068(2) 0.0239(13) -0.0124(14) -0.0013(11) 0.0070(13) C44B 0.0291(14) 0.068(2) 0.0239(13) -0.0124(14) -0.0013(11) 0.0070(13) C45B 0.0291(14) 0.068(2) 0.0239(13) -0.0124(14) -0.0013(11) 0.0070(13) C46B 0.0291(14) 0.068(2) 0.0239(13) -0.0124(14) -0.0013(11) 0.0070(13) C47B 0.0254(13) 0.0577(19) 0.0195(12) 0.0001(12) -0.0033(10) -0.0002(12) C48B 0.0254(13) 0.0577(19) 0.0195(12) 0.0001(12) -0.0033(10) -0.0002(12) C49B 0.0254(13) 0.0577(19) 0.0195(12) 0.0001(12) -0.0033(10) -0.0002(12) C50B 0.0254(13) 0.0577(19) 0.0195(12) 0.0001(12) -0.0033(10) -0.0002(12) C51B 0.0254(13) 0.0577(19) 0.0195(12) 0.0001(12) -0.0033(10) -0.0002(12) C52B 0.0254(13) 0.0577(19) 0.0195(12) 0.0001(12) -0.0033(10) -0.0002(12) C53B 0.0323(14) 0.0500(18) 0.0249(13) -0.0017(13) -0.0022(11) 0.0045(12) C54B 0.0323(14) 0.0500(18) 0.0249(13) -0.0017(13) -0.0022(11) 0.0045(12) C55B 0.0323(14) 0.0500(18) 0.0249(13) -0.0017(13) -0.0022(11) 0.0045(12) C56B 0.0323(14) 0.0500(18) 0.0249(13) -0.0017(13) -0.0022(11) 0.0045(12) C57B 0.0323(14) 0.0500(18) 0.0249(13) -0.0017(13) -0.0022(11) 0.0045(12) C58B 0.0323(14) 0.0500(18) 0.0249(13) -0.0017(13) -0.0022(11) 0.0045(12) C61B 0.0467(17) 0.0535(19) 0.0268(14) 0.0022(13) -0.0042(12) 0.0124(15) C62B 0.0467(17) 0.0535(19) 0.0268(14) 0.0022(13) -0.0042(12) 0.0124(15) C63B 0.0467(17) 0.0535(19) 0.0268(14) 0.0022(13) -0.0042(12) 0.0124(15) C64B 0.0467(17) 0.0535(19) 0.0268(14) 0.0022(13) -0.0042(12) 0.0124(15) C65B 0.0467(17) 0.0535(19) 0.0268(14) 0.0022(13) -0.0042(12) 0.0124(15) C66B 0.0467(17) 0.0535(19) 0.0268(14) 0.0022(13) -0.0042(12) 0.0124(15) C67B 0.0344(15) 0.0410(17) 0.0408(16) -0.0046(13) -0.0095(12) 0.0082(13) C68B 0.0344(15) 0.0410(17) 0.0408(16) -0.0046(13) -0.0095(12) 0.0082(13) C69B 0.0344(15) 0.0410(17) 0.0408(16) -0.0046(13) -0.0095(12) 0.0082(13) C70B 0.0344(15) 0.0410(17) 0.0408(16) -0.0046(13) -0.0095(12) 0.0082(13) C71B 0.0344(15) 0.0410(17) 0.0408(16) -0.0046(13) -0.0095(12) 0.0082(13) C72B 0.0344(15) 0.0410(17) 0.0408(16) -0.0046(13) -0.0095(12) 0.0082(13) C73B 0.0411(16) 0.0424(17) 0.0312(14) -0.0054(13) 0.0055(12) 0.0086(13) C74B 0.0411(16) 0.0424(17) 0.0312(14) -0.0054(13) 0.0055(12) 0.0086(13) C75B 0.0411(16) 0.0424(17) 0.0312(14) -0.0054(13) 0.0055(12) 0.0086(13) C76B 0.0411(16) 0.0424(17) 0.0312(14) -0.0054(13) 0.0055(12) 0.0086(13) C77B 0.0411(16) 0.0424(17) 0.0312(14) -0.0054(13) 0.0055(12) 0.0086(13) C78B 0.0411(16) 0.0424(17) 0.0312(14) -0.0054(13) 0.0055(12) 0.0086(13) O51 0.025(2) 0.049(3) 0.029(2) -0.003(2) 0.0065(18) -0.001(2) O52 0.027(2) 0.045(3) 0.039(3) -0.002(2) 0.0074(19) 0.001(2) C501 0.171(7) 0.152(7) 0.115(5) -0.002(5) -0.018(5) -0.006(5) C502 0.171(7) 0.152(7) 0.115(5) -0.002(5) -0.018(5) -0.006(5) C503 0.171(7) 0.152(7) 0.115(5) -0.002(5) -0.018(5) -0.006(5) C504 0.171(7) 0.152(7) 0.115(5) -0.002(5) -0.018(5) -0.006(5) C505 0.171(7) 0.152(7) 0.115(5) -0.002(5) -0.018(5) -0.006(5) C506 0.171(7) 0.152(7) 0.115(5) -0.002(5) -0.018(5) -0.006(5) C511 0.118(5) 0.208(8) 0.064(3) 0.018(5) -0.002(3) 0.035(5) C512 0.118(5) 0.208(8) 0.064(3) 0.018(5) -0.002(3) 0.035(5) C513 0.118(5) 0.208(8) 0.064(3) 0.018(5) -0.002(3) 0.035(5) C514 0.118(5) 0.208(8) 0.064(3) 0.018(5) -0.002(3) 0.035(5) C515 0.118(5) 0.208(8) 0.064(3) 0.018(5) -0.002(3) 0.035(5) C516 0.118(5) 0.208(8) 0.064(3) 0.018(5) -0.002(3) 0.035(5) C521 0.117(4) 0.095(4) 0.077(3) 0.003(3) 0.000(3) -0.034(3) C522 0.117(4) 0.095(4) 0.077(3) 0.003(3) 0.000(3) -0.034(3) C523 0.117(4) 0.095(4) 0.077(3) 0.003(3) 0.000(3) -0.034(3) C524 0.117(4) 0.095(4) 0.077(3) 0.003(3) 0.000(3) -0.034(3) C525 0.117(4) 0.095(4) 0.077(3) 0.003(3) 0.000(3) -0.034(3) C526 0.117(4) 0.095(4) 0.077(3) 0.003(3) 0.000(3) -0.034(3) C531 0.090(4) 0.176(7) 0.121(5) -0.008(5) -0.014(4) -0.010(4) C532 0.090(4) 0.176(7) 0.121(5) -0.008(5) -0.014(4) -0.010(4) C533 0.090(4) 0.176(7) 0.121(5) -0.008(5) -0.014(4) -0.010(4) C534 0.090(4) 0.176(7) 0.121(5) -0.008(5) -0.014(4) -0.010(4) C535 0.090(4) 0.176(7) 0.121(5) -0.008(5) -0.014(4) -0.010(4) C536 0.090(4) 0.176(7) 0.121(5) -0.008(5) -0.014(4) -0.010(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O1 2.327(4) . ? La1 O2 2.368(4) . ? La1 O52 2.450(5) . ? La1 O51 2.489(4) . ? La1 O40 2.663(5) . ? La1 O3 2.671(4) . ? La1 N1 2.718(4) . ? La1 La2 4.0412(5) . ? N1 C15 1.358(8) . ? N1 C11 1.359(7) . ? O1 C2 1.339(7) . ? O2 C22 1.310(7) . ? O3 C34 1.415(9) . ? O3 C31 1.473(9) . ? Si1 C47 1.885(8) . ? Si1 C3 1.889(6) . ? Si1 C53 1.897(8) . ? Si1 C41 1.926(10) . ? Si4 C61 1.871(9) . ? Si4 C67 1.872(7) . ? Si4 C23 1.873(6) . ? Si4 C73 1.872(6) . ? C1 C2 1.394(7) . ? C1 C9 1.417(7) . ? C1 C11 1.507(8) . ? C2 C3 1.432(7) . ? C3 C4 1.382(7) . ? C4 C10 1.411(7) . ? C4 H4 0.95 . ? C5 C6 1.377(8) . ? C5 C10 1.418(7) . ? C5 H5 0.95 . ? C6 C7 1.403(9) . ? C6 H6 0.95 . ? C7 C8 1.372(8) . ? C7 H7 0.95 . ? C8 C9 1.428(7) . ? C8 H8 0.95 . ? C9 C10 1.426(9) . ? C11 C12 1.397(8) . ? C12 C13 1.385(9) . ? C12 H12 0.95 . ? C13 C14 1.359(9) . ? C13 H13 0.95 . ? C14 C15 1.402(8) . ? C14 H14 0.95 . ? C15 C21 1.498(8) . ? C21 C22 1.413(8) . ? C21 C29 1.425(8) . ? C22 C23 1.435(7) . ? C23 C24 1.388(7) . ? C24 C30 1.428(7) . ? C24 H24 0.95 . ? C25 C26 1.381(8) . ? C25 C30 1.408(7) . ? C25 H25 0.95 . ? C26 C27 1.410(8) . ? C26 H26 0.95 . ? C27 C28 1.373(9) . ? C27 H27 0.95 . ? C28 C29 1.427(8) . ? C28 H28 0.95 . ? C29 C30 1.434(9) . ? C31 C32 1.488(11) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.513(13) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 C34 1.467(13) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C41 C46 1.398(10) . ? C41 C42 1.409(9) . ? C42 C43 1.422(10) . ? C42 H42 0.95 . ? C43 C44 1.373(10) . ? C43 H43 0.95 . ? C44 C45 1.389(10) . ? C44 H44 0.95 . ? C45 C46 1.439(10) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? C47 C48 1.383(8) . ? C47 C52 1.389(9) . ? C48 C49 1.391(8) . ? C48 H48 0.95 . ? C49 C50 1.380(9) . ? C49 H49 0.95 . ? C50 C51 1.380(9) . ? C50 H50 0.95 . ? C51 C52 1.387(8) . ? C51 H51 0.95 . ? C52 H52 0.95 . ? C53 C58 1.391(9) . ? C53 C54 1.400(8) . ? C54 C55 1.379(9) . ? C54 H54 0.95 . ? C55 C56 1.368(9) . ? C55 H55 0.95 . ? C56 C57 1.388(8) . ? C56 H56 0.95 . ? C57 C58 1.386(9) . ? C57 H57 0.95 . ? C58 H58 0.95 . ? C61 C66 1.393(10) . ? C61 C62 1.400(9) . ? C62 C63 1.395(10) . ? C62 H62 0.95 . ? C63 C64 1.407(10) . ? C63 H63 0.95 . ? C64 C65 1.386(10) . ? C64 H64 0.95 . ? C65 C66 1.379(10) . ? C65 H65 0.95 . ? C66 H66 0.95 . ? C67 C72 1.403(8) . ? C67 C68 1.402(7) . ? C68 C69 1.396(8) . ? C68 H68 0.95 . ? C69 C70 1.379(8) . ? C69 H69 0.95 . ? C70 C71 1.394(7) . ? C70 H70 0.95 . ? C71 C72 1.397(8) . ? C71 H71 0.95 . ? C72 H72 0.95 . ? C73 C78 1.393(7) . ? C73 C74 1.393(7) . ? C74 C75 1.389(7) . ? C74 H74 0.95 . ? C75 C76 1.389(7) . ? C75 H75 0.95 . ? C76 C77 1.372(8) . ? C76 H76 0.95 . ? C77 C78 1.386(7) . ? C77 H77 0.95 . ? C78 H78 0.95 . ? La2 O2B 2.352(4) . ? La2 O1B 2.362(4) . ? La2 O51 2.383(4) . ? La2 O52 2.430(4) . ? La2 O40B 2.699(6) . ? La2 N1B 2.706(5) . ? N1B C15B 1.353(7) . ? N1B C11B 1.370(8) . ? O1B C2B 1.339(7) . ? O2B C22B 1.328(6) . ? Si1B C47B 1.873(6) . ? Si1B C41B 1.873(6) . ? Si1B C3B 1.876(6) . ? Si1B C53B 1.885(7) . ? Si2B C61B 1.875(7) . ? Si2B C73B 1.877(7) . ? Si2B C23B 1.892(6) . ? Si2B C67B 1.898(7) . ? C1B C2B 1.404(7) . ? C1B C9B 1.423(8) . ? C1B C11B 1.504(8) . ? C2B C3B 1.443(7) . ? C3B C4B 1.388(8) . ? C4B C10B 1.414(8) . ? C4B H4B 0.95 . ? C5B C6B 1.382(9) . ? C5B C10B 1.410(8) . ? C5B H5B 0.95 . ? C6B C7B 1.408(8) . ? C6B H6B 0.95 . ? C7B C8B 1.378(8) . ? C7B H7B 0.95 . ? C8B C9B 1.417(8) . ? C8B H8B 0.95 . ? C9B C10B 1.433(8) . ? C11B C12B 1.393(9) . ? C12B C13B 1.376(9) . ? C12B H12B 0.95 . ? C13B C14B 1.378(9) . ? C13B H13B 0.95 . ? C14B C15B 1.407(8) . ? C14B H14B 0.95 . ? C15B C21B 1.508(8) . ? C21B C22B 1.409(7) . ? C21B C29B 1.435(7) . ? C22B C23B 1.428(7) . ? C23B C24B 1.397(7) . ? C24B C30B 1.427(7) . ? C24B H24B 0.95 . ? C25B C26B 1.379(8) . ? C25B C30B 1.421(7) . ? C25B H25B 0.95 . ? C26B C27B 1.417(8) . ? C26B H26B 0.95 . ? C27B C28B 1.373(8) . ? C27B H27B 0.95 . ? C28B C29B 1.431(7) . ? C28B H28B 0.95 . ? C29B C30B 1.400(8) . ? C41B C46B 1.392(8) . ? C41B C42B 1.401(7) . ? C42B C43B 1.394(7) . ? C42B H42B 0.95 . ? C43B C44B 1.388(8) . ? C43B H43B 0.95 . ? C44B C45B 1.385(7) . ? C44B H44B 0.95 . ? C45B C46B 1.395(7) . ? C45B H45B 0.95 . ? C46B H46B 0.95 . ? C47B C52B 1.395(7) . ? C47B C48B 1.404(7) . ? C48B C49B 1.383(7) . ? C48B H48B 0.95 . ? C49B C50B 1.398(7) . ? C49B H49B 0.95 . ? C50B C51B 1.375(8) . ? C50B H50B 0.95 . ? C51B C52B 1.400(7) . ? C51B H51B 0.95 . ? C52B H52B 0.95 . ? C53B C54B 1.389(8) . ? C53B C58B 1.404(8) . ? C54B C55B 1.387(8) . ? C54B H54B 0.95 . ? C55B C56B 1.387(8) . ? C55B H55B 0.95 . ? C56B C57B 1.391(8) . ? C56B H56B 0.95 . ? C57B C58B 1.401(8) . ? C57B H57B 0.95 . ? C58B H58B 0.95 . ? C61B C66B 1.398(8) . ? C61B C62B 1.399(7) . ? C62B C63B 1.392(8) . ? C62B H62B 0.95 . ? C63B C64B 1.383(8) . ? C63B H63B 0.95 . ? C64B C65B 1.381(8) . ? C64B H64B 0.95 . ? C65B C66B 1.388(8) . ? C65B H65B 0.95 . ? C66B H66B 0.95 . ? C67B C68B 1.393(8) . ? C67B C72B 1.398(8) . ? C68B C69B 1.399(8) . ? C68B H68B 0.95 . ? C69B C70B 1.386(8) . ? C69B H69B 0.95 . ? C70B C71B 1.381(8) . ? C70B H70B 0.95 . ? C71B C72B 1.395(8) . ? C71B H71B 0.95 . ? C72B H72B 0.95 . ? C73B C78B 1.390(8) . ? C73B C74B 1.396(7) . ? C74B C75B 1.387(7) . ? C74B H74B 0.95 . ? C75B C76B 1.379(8) . ? C75B H75B 0.95 . ? C76B C77B 1.382(8) . ? C76B H76B 0.95 . ? C77B C78B 1.391(8) . ? C77B H77B 0.95 . ? C78B H78B 0.95 . ? C501 C506 1.374(12) . ? C501 C502 1.391(11) . ? C501 H501 0.95 . ? C502 C503 1.357(13) . ? C502 H502 0.95 . ? C503 C504 1.373(12) . ? C503 H503 0.95 . ? C504 C505 1.343(12) . ? C504 H504 0.95 . ? C505 C506 1.394(13) . ? C505 H505 0.95 . ? C506 H506 0.95 . ? C511 C516 1.266(12) . ? C511 C512 1.314(10) . ? C511 H511 0.95 . ? C512 C513 1.352(12) . ? C512 H512 0.95 . ? C513 C514 1.339(12) . ? C513 H513 0.95 . ? C514 C515 1.340(12) . ? C514 H514 0.95 . ? C515 C516 1.296(12) . ? C515 H515 0.95 . ? C516 H516 0.95 . ? C521 C522 1.371(10) . ? C521 C526 1.384(11) . ? C521 H521 0.95 . ? C522 C523 1.372(11) . ? C522 H522 0.95 . ? C523 C524 1.386(11) . ? C523 H523 0.95 . ? C524 C525 1.395(11) . ? C524 H524 0.95 . ? C525 C526 1.392(11) . ? C525 H525 0.95 . ? C526 H526 0.95 . ? C531 C536 1.344(12) . ? C531 C532 1.387(10) . ? C531 H531 0.95 . ? C532 C533 1.374(12) . ? C532 H532 0.95 . ? C533 C534 1.393(12) . ? C533 H533 0.95 . ? C534 C535 1.392(12) . ? C534 H534 0.95 . ? C535 C536 1.356(12) . ? C535 H535 0.95 . ? C536 H536 0.95 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 La1 O2 108.46(14) . . ? O1 La1 O52 143.63(14) . . ? O2 La1 O52 94.92(14) . . ? O1 La1 O51 81.01(14) . . ? O2 La1 O51 152.83(14) . . ? O52 La1 O51 66.51(15) . . ? O1 La1 O40 99.18(17) . . ? O2 La1 O40 127.97(18) . . ? O52 La1 O40 86.97(19) . . ? O51 La1 O40 72.95(19) . . ? O1 La1 O3 73.34(15) . . ? O2 La1 O3 70.67(14) . . ? O52 La1 O3 142.28(15) . . ? O51 La1 O3 136.05(15) . . ? O40 La1 O3 76.6(2) . . ? O1 La1 N1 72.85(14) . . ? O2 La1 N1 70.31(14) . . ? O52 La1 N1 90.20(15) . . ? O51 La1 N1 89.32(14) . . ? O40 La1 N1 161.67(19) . . ? O3 La1 N1 115.30(14) . . ? O1 La1 La2 113.79(10) . . ? O2 La1 La2 127.93(10) . . ? O52 La1 La2 33.94(10) . . ? O51 La1 La2 33.14(11) . . ? O40 La1 La2 73.47(17) . . ? O3 La1 La2 149.99(11) . . ? N1 La1 La2 94.32(10) . . ? C15 N1 C11 118.6(5) . . ? C15 N1 La1 119.6(3) . . ? C11 N1 La1 117.2(4) . . ? C2 O1 La1 123.2(3) . . ? C22 O2 La1 124.0(3) . . ? C34 O3 C31 106.2(6) . . ? C34 O3 La1 134.0(5) . . ? C31 O3 La1 113.9(4) . . ? C47 Si1 C3 109.0(3) . . ? C47 Si1 C53 106.2(3) . . ? C3 Si1 C53 113.0(3) . . ? C47 Si1 C41 108.4(4) . . ? C3 Si1 C41 107.0(3) . . ? C53 Si1 C41 113.1(4) . . ? C61 Si4 C67 108.5(4) . . ? C61 Si4 C23 109.1(4) . . ? C67 Si4 C23 110.8(2) . . ? C61 Si4 C73 106.8(3) . . ? C67 Si4 C73 110.4(3) . . ? C23 Si4 C73 111.1(2) . . ? C2 C1 C9 120.4(6) . . ? C2 C1 C11 119.5(5) . . ? C9 C1 C11 118.8(5) . . ? O1 C2 C1 122.0(5) . . ? O1 C2 C3 117.8(5) . . ? C1 C2 C3 120.1(5) . . ? C4 C3 C2 119.1(5) . . ? C4 C3 Si1 121.8(5) . . ? C2 C3 Si1 117.3(4) . . ? C3 C4 C10 121.9(6) . . ? C3 C4 H4 119 . . ? C10 C4 H4 119 . . ? C6 C5 C10 120.6(7) . . ? C6 C5 H5 119.7 . . ? C10 C5 H5 119.7 . . ? C5 C6 C7 119.8(7) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 120.8(6) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 121.3(6) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C1 C9 C10 119.6(5) . . ? C1 C9 C8 123.1(6) . . ? C10 C9 C8 117.3(5) . . ? C4 C10 C5 121.2(6) . . ? C4 C10 C9 118.7(5) . . ? C5 C10 C9 120.0(6) . . ? N1 C11 C12 121.4(6) . . ? N1 C11 C1 121.5(5) . . ? C12 C11 C1 117.1(5) . . ? C13 C12 C11 119.3(6) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 C12 119.3(6) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 120.1(6) . . ? C13 C14 H14 120 . . ? C15 C14 H14 120 . . ? N1 C15 C14 121.1(5) . . ? N1 C15 C21 121.2(5) . . ? C14 C15 C21 117.6(5) . . ? C22 C21 C29 120.1(5) . . ? C22 C21 C15 119.0(5) . . ? C29 C21 C15 119.2(5) . . ? O2 C22 C21 121.3(5) . . ? O2 C22 C23 118.4(5) . . ? C21 C22 C23 120.3(5) . . ? C24 C23 C22 119.2(5) . . ? C24 C23 Si4 121.7(4) . . ? C22 C23 Si4 118.9(4) . . ? C23 C24 C30 121.9(6) . . ? C23 C24 H24 119.1 . . ? C30 C24 H24 119.1 . . ? C26 C25 C30 121.0(6) . . ? C26 C25 H25 119.5 . . ? C30 C25 H25 119.5 . . ? C25 C26 C27 118.9(6) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? C28 C27 C26 121.5(6) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C27 C28 C29 121.2(6) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C21 C29 C28 123.4(6) . . ? C21 C29 C30 119.6(5) . . ? C28 C29 C30 116.8(5) . . ? C25 C30 C24 120.8(6) . . ? C25 C30 C29 120.5(5) . . ? C24 C30 C29 118.7(5) . . ? O3 C31 C32 107.1(7) . . ? O3 C31 H31A 110.3 . . ? C32 C31 H31A 110.3 . . ? O3 C31 H31B 110.3 . . ? C32 C31 H31B 110.3 . . ? H31A C31 H31B 108.6 . . ? C31 C32 C33 102.4(7) . . ? C31 C32 H32A 111.3 . . ? C33 C32 H32A 111.3 . . ? C31 C32 H32B 111.3 . . ? C33 C32 H32B 111.3 . . ? H32A C32 H32B 109.2 . . ? C34 C33 C32 107.0(8) . . ? C34 C33 H33A 110.3 . . ? C32 C33 H33A 110.3 . . ? C34 C33 H33B 110.3 . . ? C32 C33 H33B 110.3 . . ? H33A C33 H33B 108.6 . . ? O3 C34 C33 109.3(8) . . ? O3 C34 H34A 109.8 . . ? C33 C34 H34A 109.8 . . ? O3 C34 H34B 109.8 . . ? C33 C34 H34B 109.8 . . ? H34A C34 H34B 108.3 . . ? C46 C41 C42 113.9(9) . . ? C46 C41 Si1 125.8(8) . . ? C42 C41 Si1 120.2(6) . . ? C41 C42 C43 127.4(9) . . ? C41 C42 H42 116.3 . . ? C43 C42 H42 116.3 . . ? C44 C43 C42 112.6(9) . . ? C44 C43 H43 123.7 . . ? C42 C43 H43 123.7 . . ? C43 C44 C45 126.5(9) . . ? C43 C44 H44 116.7 . . ? C45 C44 H44 116.7 . . ? C44 C45 C46 116.0(9) . . ? C44 C45 H45 122 . . ? C46 C45 H45 122 . . ? C41 C46 C45 123.0(10) . . ? C41 C46 H46 118.5 . . ? C45 C46 H46 118.5 . . ? C48 C47 C52 116.5(7) . . ? C48 C47 Si1 121.1(6) . . ? C52 C47 Si1 122.4(5) . . ? C47 C48 C49 121.5(8) . . ? C47 C48 H48 119.3 . . ? C49 C48 H48 119.3 . . ? C50 C49 C48 121.1(7) . . ? C50 C49 H49 119.5 . . ? C48 C49 H49 119.5 . . ? C51 C50 C49 118.2(7) . . ? C51 C50 H50 120.9 . . ? C49 C50 H50 120.9 . . ? C50 C51 C52 120.2(8) . . ? C50 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C51 C52 C47 122.5(7) . . ? C51 C52 H52 118.7 . . ? C47 C52 H52 118.7 . . ? C58 C53 C54 115.7(7) . . ? C58 C53 Si1 118.9(5) . . ? C54 C53 Si1 124.9(6) . . ? C55 C54 C53 122.8(8) . . ? C55 C54 H54 118.6 . . ? C53 C54 H54 118.6 . . ? C56 C55 C54 119.5(7) . . ? C56 C55 H55 120.2 . . ? C54 C55 H55 120.2 . . ? C55 C56 C57 120.1(8) . . ? C55 C56 H56 119.9 . . ? C57 C56 H56 119.9 . . ? C58 C57 C56 119.3(8) . . ? C58 C57 H57 120.4 . . ? C56 C57 H57 120.4 . . ? C57 C58 C53 122.5(7) . . ? C57 C58 H58 118.8 . . ? C53 C58 H58 118.8 . . ? C66 C61 C62 117.4(8) . . ? C66 C61 Si4 121.3(7) . . ? C62 C61 Si4 121.0(6) . . ? C63 C62 C61 120.9(9) . . ? C63 C62 H62 119.5 . . ? C61 C62 H62 119.5 . . ? C62 C63 C64 120.2(9) . . ? C62 C63 H63 119.9 . . ? C64 C63 H63 119.9 . . ? C65 C64 C63 118.8(9) . . ? C65 C64 H64 120.6 . . ? C63 C64 H64 120.6 . . ? C66 C65 C64 120.1(9) . . ? C66 C65 H65 119.9 . . ? C64 C65 H65 119.9 . . ? C65 C66 C61 122.4(9) . . ? C65 C66 H66 118.8 . . ? C61 C66 H66 118.8 . . ? C72 C67 C68 116.9(6) . . ? C72 C67 Si4 121.8(4) . . ? C68 C67 Si4 121.1(5) . . ? C69 C68 C67 122.1(6) . . ? C69 C68 H68 119 . . ? C67 C68 H68 119 . . ? C70 C69 C68 119.4(6) . . ? C70 C69 H69 120.3 . . ? C68 C69 H69 120.3 . . ? C69 C70 C71 120.5(6) . . ? C69 C70 H70 119.8 . . ? C71 C70 H70 119.8 . . ? C70 C71 C72 119.4(6) . . ? C70 C71 H71 120.3 . . ? C72 C71 H71 120.3 . . ? C71 C72 C67 121.6(6) . . ? C71 C72 H72 119.2 . . ? C67 C72 H72 119.2 . . ? C78 C73 C74 116.6(6) . . ? C78 C73 Si4 121.4(5) . . ? C74 C73 Si4 122.0(5) . . ? C75 C74 C73 121.5(6) . . ? C75 C74 H74 119.3 . . ? C73 C74 H74 119.3 . . ? C74 C75 C76 120.2(6) . . ? C74 C75 H75 119.9 . . ? C76 C75 H75 119.9 . . ? C77 C76 C75 119.4(6) . . ? C77 C76 H76 120.3 . . ? C75 C76 H76 120.3 . . ? C76 C77 C78 119.7(6) . . ? C76 C77 H77 120.1 . . ? C78 C77 H77 120.1 . . ? C77 C78 C73 122.5(6) . . ? C77 C78 H78 118.7 . . ? C73 C78 H78 118.7 . . ? O2B La2 O1B 104.33(13) . . ? O2B La2 O51 136.88(14) . . ? O1B La2 O51 97.74(14) . . ? O2B La2 O52 96.56(15) . . ? O1B La2 O52 158.77(14) . . ? O51 La2 O52 68.49(15) . . ? O2B La2 O40B 73.86(16) . . ? O1B La2 O40B 69.49(18) . . ? O51 La2 O40B 149.23(16) . . ? O52 La2 O40B 113.85(19) . . ? O2B La2 N1B 72.11(15) . . ? O1B La2 N1B 70.95(14) . . ? O51 La2 N1B 81.07(15) . . ? O52 La2 N1B 120.21(15) . . ? O40B La2 N1B 117.98(17) . . ? O2B La2 La1 116.80(9) . . ? O1B La2 La1 132.09(10) . . ? O51 La2 La1 34.81(10) . . ? O52 La2 La1 34.27(11) . . ? O40B La2 La1 143.28(14) . . ? N1B La2 La1 98.46(10) . . ? C15B N1B C11B 119.1(5) . . ? C15B N1B La2 118.2(4) . . ? C11B N1B La2 118.5(4) . . ? C2B O1B La2 117.4(3) . . ? C22B O2B La2 121.4(3) . . ? C47B Si1B C41B 104.7(3) . . ? C47B Si1B C3B 110.3(3) . . ? C41B Si1B C3B 111.0(3) . . ? C47B Si1B C53B 109.4(3) . . ? C41B Si1B C53B 110.8(3) . . ? C3B Si1B C53B 110.4(3) . . ? C61B Si2B C73B 110.8(3) . . ? C61B Si2B C23B 112.0(3) . . ? C73B Si2B C23B 112.4(3) . . ? C61B Si2B C67B 105.5(3) . . ? C73B Si2B C67B 104.8(3) . . ? C23B Si2B C67B 110.9(3) . . ? C2B C1B C9B 120.6(5) . . ? C2B C1B C11B 118.2(5) . . ? C9B C1B C11B 120.6(5) . . ? O1B C2B C1B 122.6(5) . . ? O1B C2B C3B 116.7(5) . . ? C1B C2B C3B 120.5(6) . . ? C4B C3B C2B 118.1(5) . . ? C4B C3B Si1B 123.3(4) . . ? C2B C3B Si1B 118.3(4) . . ? C3B C4B C10B 122.7(5) . . ? C3B C4B H4B 118.6 . . ? C10B C4B H4B 118.6 . . ? C6B C5B C10B 121.1(6) . . ? C6B C5B H5B 119.5 . . ? C10B C5B H5B 119.5 . . ? C5B C6B C7B 118.8(7) . . ? C5B C6B H6B 120.6 . . ? C7B C6B H6B 120.6 . . ? C8B C7B C6B 121.3(7) . . ? C8B C7B H7B 119.3 . . ? C6B C7B H7B 119.3 . . ? C7B C8B C9B 121.4(6) . . ? C7B C8B H8B 119.3 . . ? C9B C8B H8B 119.3 . . ? C8B C9B C1B 124.0(6) . . ? C8B C9B C10B 117.0(6) . . ? C1B C9B C10B 119.0(6) . . ? C5B C10B C4B 120.5(6) . . ? C5B C10B C9B 120.4(6) . . ? C4B C10B C9B 119.1(5) . . ? N1B C11B C12B 120.7(5) . . ? N1B C11B C1B 120.6(5) . . ? C12B C11B C1B 118.7(5) . . ? C13B C12B C11B 120.5(6) . . ? C13B C12B H12B 119.8 . . ? C11B C12B H12B 119.8 . . ? C12B C13B C14B 118.8(6) . . ? C12B C13B H13B 120.6 . . ? C14B C13B H13B 120.6 . . ? C13B C14B C15B 119.9(6) . . ? C13B C14B H14B 120.1 . . ? C15B C14B H14B 120.1 . . ? N1B C15B C14B 121.1(6) . . ? N1B C15B C21B 121.3(5) . . ? C14B C15B C21B 117.7(5) . . ? C22B C21B C29B 119.6(5) . . ? C22B C21B C15B 119.5(5) . . ? C29B C21B C15B 119.4(5) . . ? O2B C22B C21B 121.9(5) . . ? O2B C22B C23B 117.5(5) . . ? C21B C22B C23B 120.6(5) . . ? C24B C23B C22B 119.0(5) . . ? C24B C23B Si2B 122.1(4) . . ? C22B C23B Si2B 118.6(4) . . ? C23B C24B C30B 121.2(5) . . ? C23B C24B H24B 119.4 . . ? C30B C24B H24B 119.4 . . ? C26B C25B C30B 120.4(6) . . ? C26B C25B H25B 119.8 . . ? C30B C25B H25B 119.8 . . ? C25B C26B C27B 119.4(5) . . ? C25B C26B H26B 120.3 . . ? C27B C26B H26B 120.3 . . ? C28B C27B C26B 120.6(6) . . ? C28B C27B H27B 119.7 . . ? C26B C27B H27B 119.7 . . ? C27B C28B C29B 120.9(6) . . ? C27B C28B H28B 119.5 . . ? C29B C28B H28B 119.5 . . ? C30B C29B C28B 118.0(5) . . ? C30B C29B C21B 119.9(5) . . ? C28B C29B C21B 122.1(6) . . ? C29B C30B C25B 120.6(5) . . ? C29B C30B C24B 119.6(5) . . ? C25B C30B C24B 119.8(5) . . ? C46B C41B C42B 116.5(6) . . ? C46B C41B Si1B 119.7(4) . . ? C42B C41B Si1B 123.6(5) . . ? C43B C42B C41B 121.8(6) . . ? C43B C42B H42B 119.1 . . ? C41B C42B H42B 119.1 . . ? C44B C43B C42B 120.3(6) . . ? C44B C43B H43B 119.9 . . ? C42B C43B H43B 119.9 . . ? C45B C44B C43B 119.0(6) . . ? C45B C44B H44B 120.5 . . ? C43B C44B H44B 120.5 . . ? C44B C45B C46B 120.1(6) . . ? C44B C45B H45B 119.9 . . ? C46B C45B H45B 119.9 . . ? C41B C46B C45B 122.2(6) . . ? C41B C46B H46B 118.9 . . ? C45B C46B H46B 118.9 . . ? C52B C47B C48B 116.0(5) . . ? C52B C47B Si1B 123.3(5) . . ? C48B C47B Si1B 120.7(4) . . ? C49B C48B C47B 123.7(6) . . ? C49B C48B H48B 118.2 . . ? C47B C48B H48B 118.2 . . ? C48B C49B C50B 118.6(6) . . ? C48B C49B H49B 120.7 . . ? C50B C49B H49B 120.7 . . ? C51B C50B C49B 119.4(6) . . ? C51B C50B H50B 120.3 . . ? C49B C50B H50B 120.3 . . ? C50B C51B C52B 121.1(6) . . ? C50B C51B H51B 119.5 . . ? C52B C51B H51B 119.5 . . ? C47B C52B C51B 121.2(6) . . ? C47B C52B H52B 119.4 . . ? C51B C52B H52B 119.4 . . ? C54B C53B C58B 116.5(6) . . ? C54B C53B Si1B 122.1(5) . . ? C58B C53B Si1B 121.3(5) . . ? C55B C54B C53B 122.6(6) . . ? C55B C54B H54B 118.7 . . ? C53B C54B H54B 118.7 . . ? C54B C55B C56B 120.1(7) . . ? C54B C55B H55B 120 . . ? C56B C55B H55B 120 . . ? C55B C56B C57B 119.2(6) . . ? C55B C56B H56B 120.4 . . ? C57B C56B H56B 120.4 . . ? C56B C57B C58B 119.8(6) . . ? C56B C57B H57B 120.1 . . ? C58B C57B H57B 120.1 . . ? C57B C58B C53B 121.7(6) . . ? C57B C58B H58B 119.2 . . ? C53B C58B H58B 119.2 . . ? C66B C61B C62B 116.4(6) . . ? C66B C61B Si2B 120.4(5) . . ? C62B C61B Si2B 123.0(5) . . ? C63B C62B C61B 121.1(6) . . ? C63B C62B H62B 119.5 . . ? C61B C62B H62B 119.5 . . ? C64B C63B C62B 121.3(6) . . ? C64B C63B H63B 119.4 . . ? C62B C63B H63B 119.4 . . ? C65B C64B C63B 118.5(6) . . ? C65B C64B H64B 120.7 . . ? C63B C64B H64B 120.7 . . ? C64B C65B C66B 120.1(6) . . ? C64B C65B H65B 119.9 . . ? C66B C65B H65B 119.9 . . ? C65B C66B C61B 122.5(6) . . ? C65B C66B H66B 118.7 . . ? C61B C66B H66B 118.7 . . ? C68B C67B C72B 116.8(6) . . ? C68B C67B Si2B 122.7(5) . . ? C72B C67B Si2B 120.3(5) . . ? C67B C68B C69B 121.7(6) . . ? C67B C68B H68B 119.2 . . ? C69B C68B H68B 119.2 . . ? C70B C69B C68B 120.3(7) . . ? C70B C69B H69B 119.8 . . ? C68B C69B H69B 119.8 . . ? C71B C70B C69B 118.9(7) . . ? C71B C70B H70B 120.5 . . ? C69B C70B H70B 120.5 . . ? C70B C71B C72B 120.5(6) . . ? C70B C71B H71B 119.7 . . ? C72B C71B H71B 119.7 . . ? C71B C72B C67B 121.7(7) . . ? C71B C72B H72B 119.1 . . ? C67B C72B H72B 119.1 . . ? C78B C73B C74B 117.3(6) . . ? C78B C73B Si2B 123.7(5) . . ? C74B C73B Si2B 119.0(5) . . ? C75B C74B C73B 121.9(7) . . ? C75B C74B H74B 119 . . ? C73B C74B H74B 119 . . ? C76B C75B C74B 119.5(6) . . ? C76B C75B H75B 120.3 . . ? C74B C75B H75B 120.3 . . ? C75B C76B C77B 120.0(6) . . ? C75B C76B H76B 120 . . ? C77B C76B H76B 120 . . ? C76B C77B C78B 120.1(7) . . ? C76B C77B H77B 120 . . ? C78B C77B H77B 120 . . ? C73B C78B C77B 121.2(6) . . ? C73B C78B H78B 119.4 . . ? C77B C78B H78B 119.4 . . ? La2 O51 La1 112.05(18) . . ? La2 O52 La1 111.79(18) . . ? C506 C501 C502 118.8(17) . . ? C506 C501 H501 120.6 . . ? C502 C501 H501 120.6 . . ? C503 C502 C501 118.6(17) . . ? C503 C502 H502 120.7 . . ? C501 C502 H502 120.7 . . ? C502 C503 C504 119.6(18) . . ? C502 C503 H503 120.2 . . ? C504 C503 H503 120.2 . . ? C505 C504 C503 124.8(18) . . ? C505 C504 H504 117.6 . . ? C503 C504 H504 117.6 . . ? C504 C505 C506 113.7(17) . . ? C504 C505 H505 123.1 . . ? C506 C505 H505 123.1 . . ? C501 C506 C505 123.4(18) . . ? C501 C506 H506 118.3 . . ? C505 C506 H506 118.3 . . ? C516 C511 C512 118.7(17) . . ? C516 C511 H511 120.6 . . ? C512 C511 H511 120.6 . . ? C511 C512 C513 120.3(16) . . ? C511 C512 H512 119.8 . . ? C513 C512 H512 119.8 . . ? C514 C513 C512 117.9(16) . . ? C514 C513 H513 121 . . ? C512 C513 H513 121 . . ? C513 C514 C515 120.1(16) . . ? C513 C514 H514 120 . . ? C515 C514 H514 120 . . ? C516 C515 C514 117.4(16) . . ? C516 C515 H515 121.3 . . ? C514 C515 H515 121.3 . . ? C511 C516 C515 124.9(18) . . ? C511 C516 H516 117.5 . . ? C515 C516 H516 117.5 . . ? C522 C521 C526 120.7(13) . . ? C522 C521 H521 119.6 . . ? C526 C521 H521 119.6 . . ? C521 C522 C523 119.9(12) . . ? C521 C522 H522 120.1 . . ? C523 C522 H522 120.1 . . ? C522 C523 C524 121.7(12) . . ? C522 C523 H523 119.2 . . ? C524 C523 H523 119.2 . . ? C523 C524 C525 117.5(12) . . ? C523 C524 H524 121.2 . . ? C525 C524 H524 121.2 . . ? C526 C525 C524 121.3(12) . . ? C526 C525 H525 119.3 . . ? C524 C525 H525 119.3 . . ? C521 C526 C525 118.7(12) . . ? C521 C526 H526 120.6 . . ? C525 C526 H526 120.6 . . ? C536 C531 C532 121.9(15) . . ? C536 C531 H531 119.1 . . ? C532 C531 H531 119.1 . . ? C533 C532 C531 120.3(14) . . ? C533 C532 H532 119.8 . . ? C531 C532 H532 119.8 . . ? C532 C533 C534 116.9(14) . . ? C532 C533 H533 121.5 . . ? C534 C533 H533 121.5 . . ? C535 C534 C533 121.6(14) . . ? C535 C534 H534 119.2 . . ? C533 C534 H534 119.2 . . ? C536 C535 C534 119.6(14) . . ? C536 C535 H535 120.2 . . ? C534 C535 H535 120.2 . . ? C531 C536 C535 119.4(15) . . ? C531 C536 H536 120.3 . . ? C535 C536 H536 120.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 La1 N1 C15 138.7(4) . . . . ? O2 La1 N1 C15 21.2(4) . . . . ? O52 La1 N1 C15 -74.0(4) . . . . ? O51 La1 N1 C15 -140.5(4) . . . . ? O40 La1 N1 C15 -154.9(6) . . . . ? O3 La1 N1 C15 77.2(4) . . . . ? La2 La1 N1 C15 -107.7(4) . . . . ? O1 La1 N1 C11 -17.1(4) . . . . ? O2 La1 N1 C11 -134.7(4) . . . . ? O52 La1 N1 C11 130.2(4) . . . . ? O51 La1 N1 C11 63.7(4) . . . . ? O40 La1 N1 C11 49.2(8) . . . . ? O3 La1 N1 C11 -78.6(4) . . . . ? La2 La1 N1 C11 96.5(4) . . . . ? O2 La1 O1 C2 118.4(4) . . . . ? O52 La1 O1 C2 -8.9(5) . . . . ? O51 La1 O1 C2 -35.4(4) . . . . ? O40 La1 O1 C2 -106.3(4) . . . . ? O3 La1 O1 C2 -179.3(4) . . . . ? N1 La1 O1 C2 56.7(4) . . . . ? La2 La1 O1 C2 -30.4(4) . . . . ? O1 La1 O2 C22 -123.2(4) . . . . ? O52 La1 O2 C22 28.6(4) . . . . ? O51 La1 O2 C22 -16.3(6) . . . . ? O40 La1 O2 C22 118.5(4) . . . . ? O3 La1 O2 C22 172.8(4) . . . . ? N1 La1 O2 C22 -59.9(4) . . . . ? La2 La1 O2 C22 19.9(4) . . . . ? O1 La1 O3 C34 85.8(8) . . . . ? O2 La1 O3 C34 -157.1(8) . . . . ? O52 La1 O3 C34 -84.8(8) . . . . ? O51 La1 O3 C34 28.9(9) . . . . ? O40 La1 O3 C34 -18.2(8) . . . . ? N1 La1 O3 C34 147.0(8) . . . . ? La2 La1 O3 C34 -23.1(9) . . . . ? O1 La1 O3 C31 -62.8(5) . . . . ? O2 La1 O3 C31 54.3(5) . . . . ? O52 La1 O3 C31 126.5(5) . . . . ? O51 La1 O3 C31 -119.7(5) . . . . ? O40 La1 O3 C31 -166.8(6) . . . . ? N1 La1 O3 C31 -1.6(6) . . . . ? La2 La1 O3 C31 -171.7(5) . . . . ? La1 O1 C2 C1 -50.5(5) . . . . ? La1 O1 C2 C3 125.3(4) . . . . ? C9 C1 C2 O1 173.0(5) . . . . ? C11 C1 C2 O1 -20.0(6) . . . . ? C9 C1 C2 C3 -2.7(6) . . . . ? C11 C1 C2 C3 164.2(5) . . . . ? O1 C2 C3 C4 -175.1(5) . . . . ? C1 C2 C3 C4 0.8(6) . . . . ? O1 C2 C3 Si1 19.9(5) . . . . ? C1 C2 C3 Si1 -164.2(4) . . . . ? C47 Si1 C3 C4 1.9(6) . . . . ? C53 Si1 C3 C4 119.8(5) . . . . ? C41 Si1 C3 C4 -115.1(5) . . . . ? C47 Si1 C3 C2 166.5(4) . . . . ? C53 Si1 C3 C2 -75.6(5) . . . . ? C41 Si1 C3 C2 49.5(5) . . . . ? C2 C3 C4 C10 2.9(8) . . . . ? Si1 C3 C4 C10 167.2(5) . . . . ? C10 C5 C6 C7 1.4(11) . . . . ? C5 C6 C7 C8 -1.3(12) . . . . ? C6 C7 C8 C9 -0.4(11) . . . . ? C2 C1 C9 C10 1.1(7) . . . . ? C11 C1 C9 C10 -166.0(5) . . . . ? C2 C1 C9 C8 -177.2(5) . . . . ? C11 C1 C9 C8 15.7(8) . . . . ? C7 C8 C9 C1 -179.8(6) . . . . ? C7 C8 C9 C10 1.9(9) . . . . ? C3 C4 C10 C5 178.1(6) . . . . ? C3 C4 C10 C9 -4.5(9) . . . . ? C6 C5 C10 C4 177.5(7) . . . . ? C6 C5 C10 C9 0.2(10) . . . . ? C1 C9 C10 C4 2.4(8) . . . . ? C8 C9 C10 C4 -179.1(5) . . . . ? C1 C9 C10 C5 179.9(6) . . . . ? C8 C9 C10 C5 -1.7(9) . . . . ? C15 N1 C11 C12 -3.8(8) . . . . ? La1 N1 C11 C12 152.3(5) . . . . ? C15 N1 C11 C1 175.6(5) . . . . ? La1 N1 C11 C1 -28.3(7) . . . . ? C2 C1 C11 N1 61.9(7) . . . . ? C9 C1 C11 N1 -130.9(6) . . . . ? C2 C1 C11 C12 -118.7(6) . . . . ? C9 C1 C11 C12 48.5(8) . . . . ? N1 C11 C12 C13 2.7(9) . . . . ? C1 C11 C12 C13 -176.8(6) . . . . ? C11 C12 C13 C14 0.1(10) . . . . ? C12 C13 C14 C15 -1.7(10) . . . . ? C11 N1 C15 C14 2.2(8) . . . . ? La1 N1 C15 C14 -153.3(4) . . . . ? C11 N1 C15 C21 178.5(5) . . . . ? La1 N1 C15 C21 23.1(7) . . . . ? C13 C14 C15 N1 0.5(9) . . . . ? C13 C14 C15 C21 -175.9(6) . . . . ? N1 C15 C21 C22 -58.8(6) . . . . ? C14 C15 C21 C22 117.7(5) . . . . ? N1 C15 C21 C29 136.0(5) . . . . ? C14 C15 C21 C29 -47.5(7) . . . . ? La1 O2 C22 C21 52.0(5) . . . . ? La1 O2 C22 C23 -124.7(4) . . . . ? C29 C21 C22 O2 -174.4(5) . . . . ? C15 C21 C22 O2 20.5(6) . . . . ? C29 C21 C22 C23 2.2(5) . . . . ? C15 C21 C22 C23 -162.9(5) . . . . ? O2 C22 C23 C24 178.4(5) . . . . ? C21 C22 C23 C24 1.7(6) . . . . ? O2 C22 C23 Si4 -6.7(5) . . . . ? C21 C22 C23 Si4 176.6(3) . . . . ? C61 Si4 C23 C24 -13.2(5) . . . . ? C67 Si4 C23 C24 106.1(5) . . . . ? C73 Si4 C23 C24 -130.7(5) . . . . ? C61 Si4 C23 C22 172.0(4) . . . . ? C67 Si4 C23 C22 -68.7(4) . . . . ? C73 Si4 C23 C22 54.5(4) . . . . ? C22 C23 C24 C30 -4.9(7) . . . . ? Si4 C23 C24 C30 -179.7(4) . . . . ? C30 C25 C26 C27 -0.4(9) . . . . ? C25 C26 C27 C28 2.2(10) . . . . ? C26 C27 C28 C29 -0.3(9) . . . . ? C22 C21 C29 C28 172.5(4) . . . . ? C15 C21 C29 C28 -22.4(8) . . . . ? C22 C21 C29 C30 -2.9(7) . . . . ? C15 C21 C29 C30 162.1(5) . . . . ? C27 C28 C29 C21 -178.9(5) . . . . ? C27 C28 C29 C30 -3.4(8) . . . . ? C26 C25 C30 C24 177.7(6) . . . . ? C26 C25 C30 C29 -3.3(9) . . . . ? C23 C24 C30 C25 -176.9(5) . . . . ? C23 C24 C30 C29 4.1(8) . . . . ? C21 C29 C30 C25 -179.1(5) . . . . ? C28 C29 C30 C25 5.1(8) . . . . ? C21 C29 C30 C24 -0.1(8) . . . . ? C28 C29 C30 C24 -175.9(5) . . . . ? C34 O3 C31 C32 27.1(10) . . . . ? La1 O3 C31 C32 -175.8(6) . . . . ? O3 C31 C32 C33 -28.0(11) . . . . ? C31 C32 C33 C34 19.0(12) . . . . ? C31 O3 C34 C33 -14.5(11) . . . . ? La1 O3 C34 C33 -164.8(7) . . . . ? C32 C33 C34 O3 -3.1(13) . . . . ? C47 Si1 C41 C46 65.5(9) . . . . ? C3 Si1 C41 C46 -177.1(7) . . . . ? C53 Si1 C41 C46 -52.0(9) . . . . ? C47 Si1 C41 C42 -111.0(7) . . . . ? C3 Si1 C41 C42 6.4(7) . . . . ? C53 Si1 C41 C42 131.5(6) . . . . ? C46 C41 C42 C43 3.3(11) . . . . ? Si1 C41 C42 C43 -179.9(7) . . . . ? C41 C42 C43 C44 2.7(11) . . . . ? C42 C43 C44 C45 -6.5(13) . . . . ? C43 C44 C45 C46 4.0(14) . . . . ? C42 C41 C46 C45 -6.1(12) . . . . ? Si1 C41 C46 C45 177.3(7) . . . . ? C44 C45 C46 C41 3.0(14) . . . . ? C3 Si1 C47 C48 -67.2(7) . . . . ? C53 Si1 C47 C48 170.7(6) . . . . ? C41 Si1 C47 C48 48.9(7) . . . . ? C3 Si1 C47 C52 110.3(7) . . . . ? C53 Si1 C47 C52 -11.8(8) . . . . ? C41 Si1 C47 C52 -133.6(7) . . . . ? C52 C47 C48 C49 0.7(10) . . . . ? Si1 C47 C48 C49 178.4(6) . . . . ? C47 C48 C49 C50 -1.1(11) . . . . ? C48 C49 C50 C51 2.0(12) . . . . ? C49 C50 C51 C52 -2.7(12) . . . . ? C50 C51 C52 C47 2.5(13) . . . . ? C48 C47 C52 C51 -1.4(12) . . . . ? Si1 C47 C52 C51 -179.0(6) . . . . ? C47 Si1 C53 C58 84.8(7) . . . . ? C3 Si1 C53 C58 -34.7(7) . . . . ? C41 Si1 C53 C58 -156.5(6) . . . . ? C47 Si1 C53 C54 -87.2(7) . . . . ? C3 Si1 C53 C54 153.3(6) . . . . ? C41 Si1 C53 C54 31.5(8) . . . . ? C58 C53 C54 C55 2.8(10) . . . . ? Si1 C53 C54 C55 175.0(6) . . . . ? C53 C54 C55 C56 -0.9(10) . . . . ? C54 C55 C56 C57 -1.5(11) . . . . ? C55 C56 C57 C58 1.8(12) . . . . ? C56 C57 C58 C53 0.2(12) . . . . ? C54 C53 C58 C57 -2.4(11) . . . . ? Si1 C53 C58 C57 -175.1(6) . . . . ? C67 Si4 C61 C66 -37.1(12) . . . . ? C23 Si4 C61 C66 83.7(11) . . . . ? C73 Si4 C61 C66 -156.1(10) . . . . ? C67 Si4 C61 C62 149.8(8) . . . . ? C23 Si4 C61 C62 -89.5(9) . . . . ? C73 Si4 C61 C62 30.8(10) . . . . ? C66 C61 C62 C63 -0.3(13) . . . . ? Si4 C61 C62 C63 173.1(10) . . . . ? C61 C62 C63 C64 3.7(14) . . . . ? C62 C63 C64 C65 -3.5(18) . . . . ? C63 C64 C65 C66 0(2) . . . . ? C64 C65 C66 C61 4(2) . . . . ? C62 C61 C66 C65 -3.4(19) . . . . ? Si4 C61 C66 C65 -176.7(11) . . . . ? C61 Si4 C67 C72 131.2(6) . . . . ? C23 Si4 C67 C72 11.5(6) . . . . ? C73 Si4 C67 C72 -112.0(6) . . . . ? C61 Si4 C67 C68 -53.1(7) . . . . ? C23 Si4 C67 C68 -172.8(5) . . . . ? C73 Si4 C67 C68 63.6(6) . . . . ? C72 C67 C68 C69 1.5(9) . . . . ? Si4 C67 C68 C69 -174.3(5) . . . . ? C67 C68 C69 C70 -1.6(9) . . . . ? C68 C69 C70 C71 -0.8(10) . . . . ? C69 C70 C71 C72 3.3(10) . . . . ? C70 C71 C72 C67 -3.4(10) . . . . ? C68 C67 C72 C71 1.1(10) . . . . ? Si4 C67 C72 C71 176.9(5) . . . . ? C61 Si4 C73 C78 -90.3(7) . . . . ? C67 Si4 C73 C78 151.9(6) . . . . ? C23 Si4 C73 C78 28.6(7) . . . . ? C61 Si4 C73 C74 88.7(7) . . . . ? C67 Si4 C73 C74 -29.1(6) . . . . ? C23 Si4 C73 C74 -152.4(5) . . . . ? C78 C73 C74 C75 0.6(9) . . . . ? Si4 C73 C74 C75 -178.5(5) . . . . ? C73 C74 C75 C76 1.2(9) . . . . ? C74 C75 C76 C77 -1.3(10) . . . . ? C75 C76 C77 C78 -0.4(11) . . . . ? C76 C77 C78 C73 2.3(11) . . . . ? C74 C73 C78 C77 -2.3(10) . . . . ? Si4 C73 C78 C77 176.7(6) . . . . ? O1 La1 La2 O2B -143.86(16) . . . . ? O2 La1 La2 O2B 74.67(17) . . . . ? O52 La1 La2 O2B 59.1(2) . . . . ? O51 La1 La2 O2B -134.9(2) . . . . ? O40 La1 La2 O2B -50.94(18) . . . . ? O3 La1 La2 O2B -46.0(3) . . . . ? N1 La1 La2 O2B 142.99(16) . . . . ? O1 La1 La2 O1B 2.22(17) . . . . ? O2 La1 La2 O1B -139.24(18) . . . . ? O52 La1 La2 O1B -154.8(2) . . . . ? O51 La1 La2 O1B 11.2(2) . . . . ? O40 La1 La2 O1B 95.15(19) . . . . ? O3 La1 La2 O1B 100.1(3) . . . . ? N1 La1 La2 O1B -70.92(17) . . . . ? O1 La1 La2 O51 -8.9(2) . . . . ? O2 La1 La2 O51 -150.4(2) . . . . ? O52 La1 La2 O51 -166.0(3) . . . . ? O40 La1 La2 O51 84.0(2) . . . . ? O3 La1 La2 O51 88.9(3) . . . . ? N1 La1 La2 O51 -82.1(2) . . . . ? O1 La1 La2 O52 157.1(2) . . . . ? O2 La1 La2 O52 15.6(2) . . . . ? O51 La1 La2 O52 166.0(3) . . . . ? O40 La1 La2 O52 -110.0(2) . . . . ? O3 La1 La2 O52 -105.1(3) . . . . ? N1 La1 La2 O52 83.9(2) . . . . ? O1 La1 La2 O40B 117.1(2) . . . . ? O2 La1 La2 O40B -24.3(3) . . . . ? O52 La1 La2 O40B -39.9(3) . . . . ? O51 La1 La2 O40B 126.1(3) . . . . ? O40 La1 La2 O40B -149.9(3) . . . . ? O3 La1 La2 O40B -145.0(3) . . . . ? N1 La1 La2 O40B 44.0(2) . . . . ? O1 La1 La2 N1B -69.69(15) . . . . ? O2 La1 La2 N1B 148.84(16) . . . . ? O52 La1 La2 N1B 133.2(2) . . . . ? O51 La1 La2 N1B -60.7(2) . . . . ? O40 La1 La2 N1B 23.23(18) . . . . ? O3 La1 La2 N1B 28.2(2) . . . . ? N1 La1 La2 N1B -142.84(15) . . . . ? O2B La2 N1B C15B 21.6(4) . . . . ? O1B La2 N1B C15B 134.4(4) . . . . ? O51 La2 N1B C15B -124.2(4) . . . . ? O52 La2 N1B C15B -65.6(4) . . . . ? O40B La2 N1B C15B 81.5(4) . . . . ? La1 La2 N1B C15B -93.9(4) . . . . ? O2B La2 N1B C11B -135.2(4) . . . . ? O1B La2 N1B C11B -22.5(4) . . . . ? O51 La2 N1B C11B 79.0(4) . . . . ? O52 La2 N1B C11B 137.6(4) . . . . ? O40B La2 N1B C11B -75.4(5) . . . . ? La1 La2 N1B C11B 109.3(4) . . . . ? O2B La2 O1B C2B 128.2(3) . . . . ? O51 La2 O1B C2B -14.5(4) . . . . ? O52 La2 O1B C2B -62.3(6) . . . . ? O40B La2 O1B C2B -165.5(4) . . . . ? N1B La2 O1B C2B 63.2(3) . . . . ? La1 La2 O1B C2B -20.9(4) . . . . ? O1B La2 O2B C22B -123.6(4) . . . . ? O51 La2 O2B C22B -5.1(5) . . . . ? O52 La2 O2B C22B 60.2(4) . . . . ? O40B La2 O2B C22B 173.2(4) . . . . ? N1B La2 O2B C22B -59.4(4) . . . . ? La1 La2 O2B C22B 31.1(4) . . . . ? La2 O1B C2B C1B -60.5(5) . . . . ? La2 O1B C2B C3B 115.7(4) . . . . ? C9B C1B C2B O1B 175.5(5) . . . . ? C11B C1B C2B O1B -12.9(6) . . . . ? C9B C1B C2B C3B -0.6(6) . . . . ? C11B C1B C2B C3B 170.9(5) . . . . ? O1B C2B C3B C4B -176.1(5) . . . . ? C1B C2B C3B C4B 0.2(6) . . . . ? O1B C2B C3B Si1B 9.6(5) . . . . ? C1B C2B C3B Si1B -174.1(4) . . . . ? C47B Si1B C3B C4B 5.3(5) . . . . ? C41B Si1B C3B C4B -110.4(5) . . . . ? C53B Si1B C3B C4B 126.4(5) . . . . ? C47B Si1B C3B C2B 179.2(3) . . . . ? C41B Si1B C3B C2B 63.6(4) . . . . ? C53B Si1B C3B C2B -59.7(4) . . . . ? C2B C3B C4B C10B 0.9(8) . . . . ? Si1B C3B C4B C10B 174.9(4) . . . . ? C10B C5B C6B C7B -0.6(12) . . . . ? C5B C6B C7B C8B 0.3(13) . . . . ? C6B C7B C8B C9B 0.5(12) . . . . ? C7B C8B C9B C1B 177.8(7) . . . . ? C7B C8B C9B C10B -0.9(10) . . . . ? C2B C1B C9B C8B -178.9(5) . . . . ? C11B C1B C9B C8B 9.8(9) . . . . ? C2B C1B C9B C10B -0.2(8) . . . . ? C11B C1B C9B C10B -171.5(5) . . . . ? C6B C5B C10B C4B -179.3(7) . . . . ? C6B C5B C10B C9B 0.2(10) . . . . ? C3B C4B C10B C5B 177.9(6) . . . . ? C3B C4B C10B C9B -1.6(9) . . . . ? C8B C9B C10B C5B 0.6(9) . . . . ? C1B C9B C10B C5B -178.3(6) . . . . ? C8B C9B C10B C4B -179.9(6) . . . . ? C1B C9B C10B C4B 1.2(9) . . . . ? C15B N1B C11B C12B -1.8(9) . . . . ? La2 N1B C11B C12B 154.8(5) . . . . ? C15B N1B C11B C1B 178.4(5) . . . . ? La2 N1B C11B C1B -25.0(7) . . . . ? C2B C1B C11B N1B 58.4(7) . . . . ? C9B C1B C11B N1B -130.1(6) . . . . ? C2B C1B C11B C12B -121.3(6) . . . . ? C9B C1B C11B C12B 50.2(8) . . . . ? N1B C11B C12B C13B 0.6(10) . . . . ? C1B C11B C12B C13B -179.6(6) . . . . ? C11B C12B C13B C14B 0.5(10) . . . . ? C12B C13B C14B C15B -0.5(10) . . . . ? C11B N1B C15B C14B 1.8(8) . . . . ? La2 N1B C15B C14B -154.9(5) . . . . ? C11B N1B C15B C21B -179.8(5) . . . . ? La2 N1B C15B C21B 23.5(7) . . . . ? C13B C14B C15B N1B -0.7(9) . . . . ? C13B C14B C15B C21B -179.1(6) . . . . ? N1B C15B C21B C22B -59.8(7) . . . . ? C14B C15B C21B C22B 118.6(5) . . . . ? N1B C15B C21B C29B 134.4(6) . . . . ? C14B C15B C21B C29B -47.2(7) . . . . ? La2 O2B C22B C21B 51.8(5) . . . . ? La2 O2B C22B C23B -125.0(4) . . . . ? C29B C21B C22B O2B -174.3(5) . . . . ? C15B C21B C22B O2B 19.9(6) . . . . ? C29B C21B C22B C23B 2.4(5) . . . . ? C15B C21B C22B C23B -163.3(5) . . . . ? O2B C22B C23B C24B 177.6(5) . . . . ? C21B C22B C23B C24B 0.7(6) . . . . ? O2B C22B C23B Si2B -9.6(5) . . . . ? C21B C22B C23B Si2B 173.5(4) . . . . ? C61B Si2B C23B C24B -125.1(5) . . . . ? C73B Si2B C23B C24B 109.5(5) . . . . ? C67B Si2B C23B C24B -7.5(5) . . . . ? C61B Si2B C23B C22B 62.3(4) . . . . ? C73B Si2B C23B C22B -63.2(4) . . . . ? C67B Si2B C23B C22B 179.9(4) . . . . ? C22B C23B C24B C30B -3.1(7) . . . . ? Si2B C23B C24B C30B -175.7(4) . . . . ? C30B C25B C26B C27B -1.8(9) . . . . ? C25B C26B C27B C28B 2.7(9) . . . . ? C26B C27B C28B C29B -1.7(9) . . . . ? C27B C28B C29B C30B -0.2(8) . . . . ? C27B C28B C29B C21B -179.6(5) . . . . ? C22B C21B C29B C30B -3.1(7) . . . . ? C15B C21B C29B C30B 162.6(5) . . . . ? C22B C21B C29B C28B 176.2(5) . . . . ? C15B C21B C29B C28B -18.0(8) . . . . ? C28B C29B C30B C25B 1.2(8) . . . . ? C21B C29B C30B C25B -179.4(5) . . . . ? C28B C29B C30B C24B -178.6(5) . . . . ? C21B C29B C30B C24B 0.8(8) . . . . ? C26B C25B C30B C29B -0.2(8) . . . . ? C26B C25B C30B C24B 179.7(5) . . . . ? C23B C24B C30B C29B 2.4(8) . . . . ? C23B C24B C30B C25B -177.4(5) . . . . ? C47B Si1B C41B C46B 36.8(7) . . . . ? C3B Si1B C41B C46B 155.9(6) . . . . ? C53B Si1B C41B C46B -81.0(6) . . . . ? C47B Si1B C41B C42B -137.6(6) . . . . ? C3B Si1B C41B C42B -18.6(7) . . . . ? C53B Si1B C41B C42B 104.5(6) . . . . ? C46B C41B C42B C43B 0.6(9) . . . . ? Si1B C41B C42B C43B 175.2(6) . . . . ? C41B C42B C43B C44B 0.0(10) . . . . ? C42B C43B C44B C45B -0.2(11) . . . . ? C43B C44B C45B C46B -0.2(11) . . . . ? C42B C41B C46B C45B -1.0(11) . . . . ? Si1B C41B C46B C45B -175.9(6) . . . . ? C44B C45B C46B C41B 0.8(12) . . . . ? C41B Si1B C47B C52B -119.5(6) . . . . ? C3B Si1B C47B C52B 120.9(6) . . . . ? C53B Si1B C47B C52B -0.8(7) . . . . ? C41B Si1B C47B C48B 59.6(6) . . . . ? C3B Si1B C47B C48B -59.9(6) . . . . ? C53B Si1B C47B C48B 178.4(5) . . . . ? C52B C47B C48B C49B -1.7(9) . . . . ? Si1B C47B C48B C49B 179.1(5) . . . . ? C47B C48B C49B C50B 0.6(9) . . . . ? C48B C49B C50B C51B 0.8(9) . . . . ? C49B C50B C51B C52B -1.0(10) . . . . ? C48B C47B C52B C51B 1.5(9) . . . . ? Si1B C47B C52B C51B -179.3(5) . . . . ? C50B C51B C52B C47B -0.2(10) . . . . ? C47B Si1B C53B C54B -83.4(5) . . . . ? C41B Si1B C53B C54B 31.6(6) . . . . ? C3B Si1B C53B C54B 155.0(5) . . . . ? C47B Si1B C53B C58B 100.0(5) . . . . ? C41B Si1B C53B C58B -145.0(5) . . . . ? C3B Si1B C53B C58B -21.6(6) . . . . ? C58B C53B C54B C55B 1.5(8) . . . . ? Si1B C53B C54B C55B -175.3(5) . . . . ? C53B C54B C55B C56B 0.5(8) . . . . ? C54B C55B C56B C57B -1.5(9) . . . . ? C55B C56B C57B C58B 0.4(9) . . . . ? C56B C57B C58B C53B 1.7(9) . . . . ? C54B C53B C58B C57B -2.5(9) . . . . ? Si1B C53B C58B C57B 174.3(5) . . . . ? C73B Si2B C61B C66B -175.5(6) . . . . ? C23B Si2B C61B C66B 58.2(7) . . . . ? C67B Si2B C61B C66B -62.6(7) . . . . ? C73B Si2B C61B C62B -0.6(7) . . . . ? C23B Si2B C61B C62B -126.9(6) . . . . ? C67B Si2B C61B C62B 112.3(6) . . . . ? C66B C61B C62B C63B -1.9(9) . . . . ? Si2B C61B C62B C63B -176.9(6) . . . . ? C61B C62B C63B C64B -0.4(10) . . . . ? C62B C63B C64B C65B 2.6(11) . . . . ? C63B C64B C65B C66B -2.5(12) . . . . ? C64B C65B C66B C61B 0.1(12) . . . . ? C62B C61B C66B C65B 2.0(11) . . . . ? Si2B C61B C66B C65B 177.2(6) . . . . ? C61B Si2B C67B C68B -5.4(6) . . . . ? C73B Si2B C67B C68B 111.5(5) . . . . ? C23B Si2B C67B C68B -126.9(5) . . . . ? C61B Si2B C67B C72B 180.0(5) . . . . ? C73B Si2B C67B C72B -63.0(6) . . . . ? C23B Si2B C67B C72B 58.5(6) . . . . ? C72B C67B C68B C69B 0.7(9) . . . . ? Si2B C67B C68B C69B -174.1(5) . . . . ? C67B C68B C69B C70B -0.7(9) . . . . ? C68B C69B C70B C71B -0.2(9) . . . . ? C69B C70B C71B C72B 1.1(10) . . . . ? C70B C71B C72B C67B -1.2(10) . . . . ? C68B C67B C72B C71B 0.3(9) . . . . ? Si2B C67B C72B C71B 175.2(5) . . . . ? C61B Si2B C73B C78B -100.2(6) . . . . ? C23B Si2B C73B C78B 25.9(7) . . . . ? C67B Si2B C73B C78B 146.5(6) . . . . ? C61B Si2B C73B C74B 79.1(6) . . . . ? C23B Si2B C73B C74B -154.8(5) . . . . ? C67B Si2B C73B C74B -34.2(6) . . . . ? C78B C73B C74B C75B 0.3(9) . . . . ? Si2B C73B C74B C75B -179.1(5) . . . . ? C73B C74B C75B C76B 0.2(9) . . . . ? C74B C75B C76B C77B -1.1(10) . . . . ? C75B C76B C77B C78B 1.4(10) . . . . ? C74B C73B C78B C77B 0.1(10) . . . . ? Si2B C73B C78B C77B 179.5(5) . . . . ? C76B C77B C78B C73B -0.9(10) . . . . ? O2B La2 O51 La1 67.6(3) . . . . ? O1B La2 O51 La1 -171.66(17) . . . . ? O52 La2 O51 La1 -8.41(16) . . . . ? O40B La2 O51 La1 -109.2(3) . . . . ? N1B La2 O51 La1 119.13(19) . . . . ? O1 La1 O51 La2 171.7(2) . . . . ? O2 La1 O51 La2 58.5(4) . . . . ? O52 La1 O51 La2 8.46(16) . . . . ? O40 La1 O51 La2 -85.7(2) . . . . ? O3 La1 O51 La2 -133.9(2) . . . . ? N1 La1 O51 La2 98.98(19) . . . . ? O2B La2 O52 La1 -129.58(18) . . . . ? O1B La2 O52 La1 60.6(5) . . . . ? O51 La2 O52 La1 8.53(16) . . . . ? O40B La2 O52 La1 155.20(18) . . . . ? N1B La2 O52 La1 -56.5(2) . . . . ? O1 La1 O52 La2 -37.0(3) . . . . ? O2 La1 O52 La2 -167.71(18) . . . . ? O51 La1 O52 La2 -8.28(16) . . . . ? O40 La1 O52 La2 64.4(2) . . . . ? O3 La1 O52 La2 127.9(2) . . . . ? N1 La1 O52 La2 -97.45(19) . . . . ? C506 C501 C502 C503 -0.4(15) . . . . ? C501 C502 C503 C504 1.3(16) . . . . ? C502 C503 C504 C505 -8(2) . . . . ? C503 C504 C505 C506 12(3) . . . . ? C502 C501 C506 C505 6(2) . . . . ? C504 C505 C506 C501 -11(3) . . . . ? C516 C511 C512 C513 -3.5(16) . . . . ? C511 C512 C513 C514 -3.2(15) . . . . ? C512 C513 C514 C515 6(2) . . . . ? C513 C514 C515 C516 -2(2) . . . . ? C512 C511 C516 C515 8(2) . . . . ? C514 C515 C516 C511 -6(2) . . . . ? C526 C521 C522 C523 -0.7(13) . . . . ? C521 C522 C523 C524 -1.9(13) . . . . ? C522 C523 C524 C525 4.6(15) . . . . ? C523 C524 C525 C526 -4.9(16) . . . . ? C522 C521 C526 C525 0.4(15) . . . . ? C524 C525 C526 C521 2.5(17) . . . . ? C536 C531 C532 C533 -4.3(15) . . . . ? C531 C532 C533 C534 0.4(14) . . . . ? C532 C533 C534 C535 1(2) . . . . ? C533 C534 C535 C536 1(2) . . . . ? C532 C531 C536 C535 7(2) . . . . ? C534 C535 C536 C531 -5(2) . . . . ?