Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Daniel Leznoff' _publ_contact_author_address ; Department of Chemistry Simon Fraser University Burnaby BC V5A 1S6 CANADA ; _publ_contact_author_email DLEZNOFF@SFU.CA _publ_section_title ; Synthesis and Structure of Diamido Ether Uranium(IV) and Thorium(IV) Halide Ate Complexes and their Conversion to Salt-Free Bis-Alkyl Complexes ; _publ_section_references ; Gabe, E.J.; White, P.S.; Enright, G.D. DIFRAC A Fortran 77 Control Routine for 4-Circle Diffractometers, N.R.C., Ottawa, 1995. Gabe, E.J., Le Page, Y., Charland,.J.-P., Lee, F.L. and White, P.S. (1989) J. Appl. Cryst., 22, 384-387. International Tables for X-ray Crystallography, Vol. IV, (1974) Kynoch Press, Birmingham, England. Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A. Le Page, Y., (1988) J. Appl. Cryst., 21, 983-984. Le Page, Y. and Gabe, E.J., (1979) J. Appl. Cryst., 12, 464-466. #Absorption Correction # Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. # CRYSTALS # Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. # Extinction correction # Larson, A.C. (1970), Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294 #CAMERON # Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. #ORTEP-3 version 1.073 # Farrugia, L.J., (1997) J. Appl. Cryst. 30, 565. # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 # SHELXS 86 # Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. ; loop_ _publ_author_name 'Daniel Leznoff' 'R. Batchelor' 'Farzad Haftbaradaran' 'Kimberly C. Jantunen' 'Michael J. Katz' ; G.Schatte ; data_1 _database_code_depnum_ccdc_archive 'CCDC 271009' _chemical_formula_sum ' C36 H58 Cl3 Li1 N2 O3 U1 ' _chemical_formula_moiety ' C36 H58 Cl3 Li1 N2 O3 U1 ' _chemical_formula_weight 918.19 #============================================================= # CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 #--------------------------------------------------------------------- _cell_length_a 13.266(3) _cell_angle_alpha 90 _cell_length_b 19.914(2) _cell_angle_beta 106.776(16) _cell_length_c 16.697(3) _cell_angle_gamma 90 _cell_volume 4223.3(13) _cell_formula_units_Z 4 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 14 _cell_measurement_theta_max 15 _cell_measurement_temperature 293 _exptl_crystal_description ' block ' _exptl_crystal_colour ' green ' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 3.866 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.3281 _exptl_absorpt_correction_T_max 0.6508 #========================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.70930 _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w/2\q _diffrn_ambient_temperature 293 _diffrn_reflns_number 3835 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_theta_min 2.011 _diffrn_reflns_theta_max 19.500 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 19.500 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_standards_interval_time 150 _diffrn_standards_interval_count 25 _diffrn_standards_number 2 _diffrn_standards_decay_% 2.78 #======================================= # REFINEMENT DATA # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 3693 _reflns_number_gt 1736 _reflns_threshold_expression I>2.50u(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0389 _refine_ls_number_reflns 1736 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.1884 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo) + (0.02Fo)^2^] ; _refine_ls_shift/su_max 0.000203 _refine_diff_density_max 0.53 _refine_diff_density_min -0.47 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 15 #_refine_ls_R_factor_ref 0.0390 #_reflns_number_all 3693 _refine_ls_R_factor_all 0.1603 _refine_ls_wR_factor_all 0.0467 # Number of reflections with Friedels Law is 3693 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3678 #-------------------------------------------------------- _chemical_name_systematic ; ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_data_collection ; NRC DIFRAC ; _computing_data_reduction ; NRC DIFRAC ; _computing_cell_refinement ; NRC DIFRAC ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; #========================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'U ' -10.6730 9.6540 36.0228 0.5293 23.4128 3.3253 14.9491 16.0927 4.1880 100.6130 13.3966 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'Li ' 0.0000 0.0000 1.1282 3.9546 0.7508 1.0524 0.6175 85.3906 0.4653 168.2610 0.0377 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B #===================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens U1 U 0.80031(7) 0.06021(4) 0.79774(5) 0.0464 1.0000 Uani . . . . . . Cl1 Cl 0.7018(5) 0.0225(3) 0.6391(3) 0.0886 1.0000 Uani . . . . . . Cl2 Cl 0.6814(4) 0.1712(2) 0.7466(3) 0.0752 1.0000 Uani . . . . . . Cl3 Cl 0.9176(4) -0.0497(2) 0.8254(3) 0.0701 1.0000 Uani . . . . . . O1 O 0.8902(10) 0.0810(6) 0.9444(7) 0.0667 1.0000 Uani . . . . . . O2 O 0.6408(13) 0.1738(9) 0.5291(10) 0.1273 1.0000 Uani . . . . . . O3 O 0.4599(12) 0.1073(9) 0.5776(10) 0.1179 1.0000 Uani . . . . . . N1 N 0.7092(11) 0.0269(6) 0.8801(9) 0.0526 1.0000 Uani . . . . . . N2 N 0.9416(12) 0.1218(7) 0.8128(9) 0.0498 1.0000 Uani . . . . . . C1 C 0.7534(15) 0.0227(9) 0.9732(12) 0.070(6) 1.0000 Uiso . . . . . . C2 C 0.8309(16) 0.0763(9) 1.0026(13) 0.088(7) 1.0000 Uiso . . . . . . C3 C 0.9743(16) 0.1264(10) 0.9634(12) 0.077(7) 1.0000 Uiso . . . . . . C4 C 1.0217(16) 0.1246(10) 0.8924(12) 0.072(6) 1.0000 Uiso . . . . . . C5 C 0.6045(16) 0.0002(9) 0.8534(11) 0.052(5) 1.0000 Uiso . . . . . . C6 C 0.5893(15) -0.0675(10) 0.8289(11) 0.068(6) 1.0000 Uiso . . . . . . C7 C 0.4847(19) -0.0926(11) 0.8029(13) 0.095(8) 1.0000 Uiso . . . . . . C8 C 0.3999(19) -0.0513(12) 0.8010(12) 0.104(7) 1.0000 Uiso . . . . . . C9 C 0.4145(19) 0.0152(11) 0.8284(13) 0.094(7) 1.0000 Uiso . . . . . . C10 C 0.5169(16) 0.0401(9) 0.8532(11) 0.063(6) 1.0000 Uiso . . . . . . C11 C 0.9727(14) 0.1588(9) 0.7486(10) 0.046(5) 1.0000 Uiso . . . . . . C12 C 1.0031(13) 0.1238(8) 0.6884(10) 0.043(5) 1.0000 Uiso . . . . . . C13 C 1.0361(15) 0.1558(9) 0.6259(12) 0.072(6) 1.0000 Uiso . . . . . . C14 C 1.0382(16) 0.2256(10) 0.6248(13) 0.088(7) 1.0000 Uiso . . . . . . C15 C 1.0077(15) 0.2617(10) 0.6849(12) 0.073(7) 1.0000 Uiso . . . . . . C16 C 0.9726(15) 0.2316(9) 0.7458(11) 0.060(6) 1.0000 Uiso . . . . . . C17 C 0.733(2) 0.2130(14) 0.5410(17) 0.158(12) 1.0000 Uiso . . . . . . C18 C 0.754(3) 0.2151(15) 0.461(2) 0.193(14) 1.0000 Uiso . . . . . . C19 C 0.694(3) 0.1644(19) 0.410(2) 0.25(2) 1.0000 Uiso . . . . . . C20 C 0.606(2) 0.1606(15) 0.4457(19) 0.165(13) 1.0000 Uiso . . . . . . C21 C 0.417(2) 0.0435(14) 0.5943(18) 0.161(13) 1.0000 Uiso . . . . . . C22 C 0.304(2) 0.0590(15) 0.5771(17) 0.166(11) 1.0000 Uiso . . . . . . C23 C 0.284(2) 0.1203(15) 0.5388(19) 0.176(13) 1.0000 Uiso . . . . . . C24 C 0.382(3) 0.1474(16) 0.532(2) 0.197(16) 1.0000 Uiso . . . . . . C25 C 0.6776(18) -0.1152(10) 0.8348(13) 0.089(7) 1.0000 Uiso . . . . . . C26 C 0.6684(19) -0.1500(11) 0.7519(14) 0.131(10) 1.0000 Uiso . . . . . . C27 C 0.6854(18) -0.1664(11) 0.9019(14) 0.127(10) 1.0000 Uiso . . . . . . C28 C 0.5289(19) 0.1114(10) 0.8844(13) 0.094(7) 1.0000 Uiso . . . . . . C29 C 0.4519(18) 0.1596(11) 0.8211(14) 0.131(10) 1.0000 Uiso . . . . . . C30 C 0.5047(18) 0.1174(11) 0.9693(14) 0.127(9) 1.0000 Uiso . . . . . . C31 C 1.0100(15) 0.0468(9) 0.6866(11) 0.070(6) 1.0000 Uiso . . . . . . C32 C 0.9812(17) 0.0134(11) 0.6027(13) 0.118(9) 1.0000 Uiso . . . . . . C33 C 1.1207(17) 0.0266(10) 0.7365(13) 0.110(9) 1.0000 Uiso . . . . . . C34 C 0.9337(17) 0.2727(10) 0.8076(13) 0.082(7) 1.0000 Uiso . . . . . . C35 C 0.8506(18) 0.3218(11) 0.7626(13) 0.128(9) 1.0000 Uiso . . . . . . C36 C 1.0309(17) 0.3079(11) 0.8670(14) 0.127(9) 1.0000 Uiso . . . . . . Li1 Li 0.603(3) 0.1249(19) 0.615(2) 0.091(13) 1.0000 Uiso . . . . . . H11 H 0.7873 -0.0195 0.9878 0.09(2) 1.0000 Uiso R . . . . . H12 H 0.6987 0.0271 0.9992 0.09(2) 1.0000 Uiso R . . . . . H21 H 0.8760 0.0661 1.0567 0.11(2) 1.0000 Uiso R . . . . . H22 H 0.7955 0.1175 1.0046 0.11(2) 1.0000 Uiso R . . . . . H31 H 1.0256 0.1140 1.0138 0.11(2) 1.0000 Uiso R . . . . . H32 H 0.9494 0.1704 0.9691 0.11(2) 1.0000 Uiso R . . . . . H41 H 1.0629 0.1639 0.8943 0.10(2) 1.0000 Uiso R . . . . . H42 H 1.0654 0.0860 0.8983 0.10(2) 1.0000 Uiso R . . . . . H71 H 0.4731 -0.1381 0.7855 0.17(4) 1.0000 Uiso R . . . . . H81 H 0.3302 -0.0686 0.7828 0.18(4) 1.0000 Uiso R . . . . . H91 H 0.3566 0.0430 0.8291 0.18(4) 1.0000 Uiso R . . . . . H131 H 1.0555 0.1302 0.5846 0.14(4) 1.0000 Uiso R . . . . . H141 H 1.0599 0.2481 0.5825 0.17(4) 1.0000 Uiso R . . . . . H151 H 1.0123 0.3093 0.6845 0.16(4) 1.0000 Uiso R . . . . . H171 H 0.7896 0.1934 0.5828 0.17(3) 1.0000 Uiso R . . . . . H172 H 0.7216 0.2575 0.5569 0.17(3) 1.0000 Uiso R . . . . . H181 H 0.8249 0.2018 0.4682 0.23(3) 1.0000 Uiso R . . . . . H182 H 0.7431 0.2587 0.4370 0.23(3) 1.0000 Uiso R . . . . . H191 H 0.7284 0.1228 0.4078 0.28(3) 1.0000 Uiso R . . . . . H192 H 0.6673 0.1820 0.3551 0.28(3) 1.0000 Uiso R . . . . . H201 H 0.5495 0.1899 0.4193 0.20(3) 1.0000 Uiso R . . . . . H202 H 0.5815 0.1155 0.4390 0.20(3) 1.0000 Uiso R . . . . . H211 H 0.4466 0.0300 0.6508 0.17(3) 1.0000 Uiso R . . . . . H212 H 0.4281 0.0093 0.5581 0.17(3) 1.0000 Uiso R . . . . . H221 H 0.2860 0.0612 0.6280 0.18(3) 1.0000 Uiso R . . . . . H222 H 0.2632 0.0253 0.5421 0.18(3) 1.0000 Uiso R . . . . . H231 H 0.2505 0.1494 0.5685 0.20(3) 1.0000 Uiso R . . . . . H232 H 0.2391 0.1142 0.4835 0.20(3) 1.0000 Uiso R . . . . . H241 H 0.3903 0.1907 0.5566 0.25(3) 1.0000 Uiso R . . . . . H242 H 0.3834 0.1510 0.4752 0.25(3) 1.0000 Uiso R . . . . . H251 H 0.7401 -0.0890 0.8489 0.17(5) 1.0000 Uiso R . . . . . H261 H 0.7256 -0.1802 0.7577 0.16(4) 1.0000 Uiso R . . . . . H262 H 0.6040 -0.1741 0.7351 0.16(4) 1.0000 Uiso R . . . . . H263 H 0.6693 -0.1171 0.7108 0.16(4) 1.0000 Uiso R . . . . . H271 H 0.7421 -0.1959 0.9028 0.14(4) 1.0000 Uiso R . . . . . H272 H 0.6988 -0.1445 0.9545 0.14(4) 1.0000 Uiso R . . . . . H273 H 0.6220 -0.1915 0.8913 0.14(4) 1.0000 Uiso R . . . . . H281 H 0.6001 0.1233 0.8906 0.14(5) 1.0000 Uiso R . . . . . H291 H 0.4617 0.2042 0.8421 0.13(3) 1.0000 Uiso R . . . . . H292 H 0.3814 0.1460 0.8149 0.13(3) 1.0000 Uiso R . . . . . H293 H 0.4656 0.1578 0.7684 0.13(3) 1.0000 Uiso R . . . . . H301 H 0.5141 0.1626 0.9881 0.13(3) 1.0000 Uiso R . . . . . H302 H 0.5507 0.0891 1.0095 0.13(3) 1.0000 Uiso R . . . . . H303 H 0.4339 0.1042 0.9624 0.13(3) 1.0000 Uiso R . . . . . H311 H 0.9567 0.0326 0.7106 0.16(5) 1.0000 Uiso R . . . . . H321 H 0.9879 -0.0339 0.6105 0.15(3) 1.0000 Uiso R . . . . . H322 H 1.0276 0.0283 0.5724 0.15(3) 1.0000 Uiso R . . . . . H323 H 0.9107 0.0240 0.5722 0.15(3) 1.0000 Uiso R . . . . . H331 H 1.1262 -0.0209 0.7362 0.12(3) 1.0000 Uiso R . . . . . H332 H 1.1365 0.0422 0.7925 0.12(3) 1.0000 Uiso R . . . . . H333 H 1.1689 0.0457 0.7105 0.12(3) 1.0000 Uiso R . . . . . H341 H 0.9012 0.2456 0.8399 0.12(5) 1.0000 Uiso R . . . . . H351 H 0.8279 0.3477 0.8019 0.11(3) 1.0000 Uiso R . . . . . H352 H 0.8796 0.3506 0.7297 0.11(3) 1.0000 Uiso R . . . . . H353 H 0.7922 0.2982 0.7272 0.11(3) 1.0000 Uiso R . . . . . H361 H 1.0101 0.3347 0.9065 0.11(3) 1.0000 Uiso R . . . . . H362 H 1.0799 0.2749 0.8956 0.11(3) 1.0000 Uiso R . . . . . H363 H 1.0629 0.3355 0.8348 0.11(3) 1.0000 Uiso 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 U1 0.0491(5) 0.0453(4) 0.0404(4) 0.0016(7) 0.0057(3) -0.0023(7) Cl1 0.091(5) 0.102(4) 0.060(4) -0.023(3) 0.002(3) -0.002(4) Cl2 0.081(5) 0.068(4) 0.071(4) 0.013(3) 0.013(3) 0.016(3) Cl3 0.074(4) 0.050(3) 0.085(4) 0.014(3) 0.022(3) 0.012(3) O1 0.058(10) 0.084(11) 0.056(9) -0.005(7) 0.011(7) -0.022(8) O2 0.119(15) 0.173(16) 0.075(12) 0.042(11) 0.002(11) -0.064(13) O3 0.065(13) 0.135(15) 0.129(15) 0.026(12) -0.011(11) -0.009(12) N1 0.047(12) 0.043(9) 0.047(11) -0.008(7) -0.018(9) 0.001(8) N2 0.058(13) 0.041(10) 0.043(11) 0.001(8) 0.004(10) 0.004(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3737(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag U1 . Cl1 . 2.700(5) yes U1 . Cl2 . 2.707(5) yes U1 . Cl3 . 2.647(5) yes U1 . O1 . 2.431(12) yes U1 . N1 . 2.181(15) yes U1 . N2 . 2.193(15) yes Cl1 . Li1 . 2.39(4) yes Cl2 . Li1 . 2.34(4) yes O1 . C2 . 1.418(19) yes O1 . C3 . 1.399(19) yes O2 . C17 . 1.42(3) yes O2 . C20 . 1.36(3) yes O2 . Li1 . 1.91(4) yes O3 . C21 . 1.45(3) yes O3 . C24 . 1.36(3) yes O3 . Li1 . 1.86(4) yes N1 . C1 . 1.497(19) yes N1 . C5 . 1.43(2) yes N2 . C4 . 1.44(2) yes N2 . C11 . 1.454(18) yes C1 . C2 . 1.47(2) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C2 . H21 . 0.950 no C2 . H22 . 0.950 no C3 . C4 . 1.49(2) yes C3 . H31 . 0.950 no C3 . H32 . 0.950 no C4 . H41 . 0.950 no C4 . H42 . 0.950 no C5 . C6 . 1.41(2) yes C5 . C10 . 1.41(2) yes C6 . C7 . 1.42(2) yes C6 . C25 . 1.49(2) yes C7 . C8 . 1.39(2) yes C7 . H71 . 0.950 no C8 . C9 . 1.40(2) yes C8 . H81 . 0.950 no C9 . C10 . 1.39(2) yes C9 . H91 . 0.950 no C10 . C28 . 1.51(2) yes C11 . C12 . 1.377(19) yes C11 . C16 . 1.45(2) yes C12 . C13 . 1.40(2) yes C12 . C31 . 1.54(2) yes C13 . C14 . 1.39(2) yes C13 . H131 . 0.950 no C14 . C15 . 1.38(2) yes C14 . H141 . 0.950 no C15 . C16 . 1.37(2) yes C15 . H151 . 0.950 no C16 . C34 . 1.52(2) yes C17 . C18 . 1.45(3) yes C17 . H171 . 0.950 no C17 . H172 . 0.950 no C18 . C19 . 1.41(4) yes C18 . H181 . 0.950 no C18 . H182 . 0.950 no C19 . C20 . 1.46(4) yes C19 . H191 . 0.950 no C19 . H192 . 0.950 no C20 . H201 . 0.950 no C20 . H202 . 0.950 no C21 . C22 . 1.47(3) yes C21 . H211 . 0.950 no C21 . H212 . 0.950 no C22 . C23 . 1.37(3) yes C22 . H221 . 0.950 no C22 . H222 . 0.950 no C23 . C24 . 1.45(3) yes C23 . H231 . 0.950 no C23 . H232 . 0.950 no C24 . H241 . 0.950 no C24 . H242 . 0.950 no C25 . C26 . 1.52(2) yes C25 . C27 . 1.50(2) yes C25 . H251 . 0.950 no C26 . H261 . 0.950 no C26 . H262 . 0.950 no C26 . H263 . 0.950 no C27 . H271 . 0.950 no C27 . H272 . 0.950 no C27 . H273 . 0.950 no C28 . C29 . 1.57(3) yes C28 . C30 . 1.55(2) yes C28 . H281 . 0.950 no C29 . H291 . 0.950 no C29 . H292 . 0.950 no C29 . H293 . 0.950 no C30 . H301 . 0.950 no C30 . H302 . 0.950 no C30 . H303 . 0.950 no C31 . C32 . 1.50(2) yes C31 . C33 . 1.52(2) yes C31 . H311 . 0.950 no C32 . H321 . 0.950 no C32 . H322 . 0.950 no C32 . H323 . 0.950 no C33 . H331 . 0.950 no C33 . H332 . 0.950 no C33 . H333 . 0.950 no C34 . C35 . 1.50(2) yes C34 . C36 . 1.55(2) yes C34 . H341 . 0.950 no C35 . H351 . 0.950 no C35 . H352 . 0.950 no C35 . H353 . 0.950 no C36 . H361 . 0.950 no C36 . H362 . 0.950 no C36 . H363 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . U1 . Cl2 . 81.06(16) yes Cl1 . U1 . Cl3 . 92.01(16) yes Cl2 . U1 . Cl3 . 171.80(15) yes Cl1 . U1 . O1 . 173.7(3) yes Cl2 . U1 . O1 . 104.5(3) yes Cl3 . U1 . O1 . 82.7(3) yes Cl1 . U1 . N1 . 109.6(4) yes Cl2 . U1 . N1 . 93.9(4) yes Cl3 . U1 . N1 . 92.5(3) yes O1 . U1 . N1 . 67.4(5) yes Cl1 . U1 . N2 . 115.1(4) yes Cl2 . U1 . N2 . 88.8(4) yes Cl3 . U1 . N2 . 90.2(4) yes O1 . U1 . N2 . 68.6(5) yes N1 . U1 . N2 . 135.2(5) yes U1 . Cl1 . Li1 . 91.0(10) yes U1 . Cl2 . Li1 . 92.0(10) yes U1 . O1 . C2 . 118.1(11) yes U1 . O1 . C3 . 117.7(10) yes C2 . O1 . C3 . 116.8(14) yes C17 . O2 . C20 . 106.1(20) yes C17 . O2 . Li1 . 125(2) yes C20 . O2 . Li1 . 126(2) yes C21 . O3 . C24 . 110(2) yes C21 . O3 . Li1 . 122(2) yes C24 . O3 . Li1 . 128(2) yes U1 . N1 . C1 . 123.3(11) yes U1 . N1 . C5 . 125.5(11) yes C1 . N1 . C5 . 110.9(14) yes U1 . N2 . C4 . 120.3(11) yes U1 . N2 . C11 . 127.9(11) yes C4 . N2 . C11 . 111.7(15) yes N1 . C1 . C2 . 109.5(15) yes N1 . C1 . H11 . 109.3 no C2 . C1 . H11 . 109.0 no N1 . C1 . H12 . 110.2 no C2 . C1 . H12 . 109.5 no H11 . C1 . H12 . 109.5 no C1 . C2 . O1 . 107.0(16) yes C1 . C2 . H21 . 110.5 no O1 . C2 . H21 . 110.1 no C1 . C2 . H22 . 109.6 no O1 . C2 . H22 . 110.2 no H21 . C2 . H22 . 109.5 no O1 . C3 . C4 . 107.2(15) yes O1 . C3 . H31 . 110.6 no C4 . C3 . H31 . 109.8 no O1 . C3 . H32 . 109.9 no C4 . C3 . H32 . 109.9 no H31 . C3 . H32 . 109.5 no C3 . C4 . N2 . 111.4(17) yes C3 . C4 . H41 . 108.9 no N2 . C4 . H41 . 109.0 no C3 . C4 . H42 . 108.7 no N2 . C4 . H42 . 109.3 no H41 . C4 . H42 . 109.5 no N1 . C5 . C6 . 119.4(17) yes N1 . C5 . C10 . 121.2(16) yes C6 . C5 . C10 . 119.4(19) yes C5 . C6 . C7 . 118.2(19) yes C5 . C6 . C25 . 123.2(19) yes C7 . C6 . C25 . 118.4(20) yes C6 . C7 . C8 . 121(2) yes C6 . C7 . H71 . 119.2 no C8 . C7 . H71 . 120.0 no C7 . C8 . C9 . 121(2) yes C7 . C8 . H81 . 120.1 no C9 . C8 . H81 . 118.6 no C8 . C9 . C10 . 118(2) yes C8 . C9 . H91 . 121.3 no C10 . C9 . H91 . 120.8 no C5 . C10 . C9 . 122.3(18) yes C5 . C10 . C28 . 121.8(20) yes C9 . C10 . C28 . 116(2) yes N2 . C11 . C12 . 119.1(15) yes N2 . C11 . C16 . 122.2(15) yes C12 . C11 . C16 . 118.7(16) yes C11 . C12 . C13 . 122.4(16) yes C11 . C12 . C31 . 123.5(15) yes C13 . C12 . C31 . 114.0(16) yes C12 . C13 . C14 . 118.5(18) yes C12 . C13 . H131 . 120.4 no C14 . C13 . H131 . 121.1 no C13 . C14 . C15 . 119.9(20) yes C13 . C14 . H141 . 119.4 no C15 . C14 . H141 . 120.7 no C14 . C15 . C16 . 122.9(19) yes C14 . C15 . H151 . 118.6 no C16 . C15 . H151 . 118.5 no C11 . C16 . C15 . 117.6(17) yes C11 . C16 . C34 . 120.8(17) yes C15 . C16 . C34 . 121.5(18) yes O2 . C17 . C18 . 106(2) yes O2 . C17 . H171 . 110.2 no C18 . C17 . H171 . 111.6 no O2 . C17 . H172 . 110.8 no C18 . C17 . H172 . 108.7 no H171 . C17 . H172 . 109.5 no C17 . C18 . C19 . 108(3) yes C17 . C18 . H181 . 108.7 no C19 . C18 . H181 . 104.1 no C17 . C18 . H182 . 111.5 no C19 . C18 . H182 . 114.5 no H181 . C18 . H182 . 109.5 no C18 . C19 . C20 . 100(3) yes C18 . C19 . H191 . 117.3 no C20 . C19 . H191 . 114.7 no C18 . C19 . H192 . 107.9 no C20 . C19 . H192 . 106.8 no H191 . C19 . H192 . 109.5 no C19 . C20 . O2 . 109(3) yes C19 . C20 . H201 . 113.3 no O2 . C20 . H201 . 110.3 no C19 . C20 . H202 . 106.6 no O2 . C20 . H202 . 107.9 no H201 . C20 . H202 . 109.5 no O3 . C21 . C22 . 102(2) yes O3 . C21 . H211 . 111.3 no C22 . C21 . H211 . 111.3 no O3 . C21 . H212 . 111.1 no C22 . C21 . H212 . 111.4 no H211 . C21 . H212 . 109.5 no C21 . C22 . C23 . 110(3) yes C21 . C22 . H221 . 109.9 no C23 . C22 . H221 . 108.0 no C21 . C22 . H222 . 109.9 no C23 . C22 . H222 . 110.0 no H221 . C22 . H222 . 109.5 no C22 . C23 . C24 . 108(3) yes C22 . C23 . H231 . 111.2 no C24 . C23 . H231 . 112.4 no C22 . C23 . H232 . 108.9 no C24 . C23 . H232 . 106.8 no H231 . C23 . H232 . 109.5 no C23 . C24 . O3 . 107(3) yes C23 . C24 . H241 . 107.3 no O3 . C24 . H241 . 108.0 no C23 . C24 . H242 . 112.9 no O3 . C24 . H242 . 111.9 no H241 . C24 . H242 . 109.5 no C6 . C25 . C26 . 112.1(19) yes C6 . C25 . C27 . 111.5(18) yes C26 . C25 . C27 . 109.9(18) yes C6 . C25 . H251 . 106.2 no C26 . C25 . H251 . 108.1 no C27 . C25 . H251 . 108.9 no C25 . C26 . H261 . 110.0 no C25 . C26 . H262 . 109.1 no H261 . C26 . H262 . 109.5 no C25 . C26 . H263 . 109.2 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no C25 . C27 . H271 . 108.4 no C25 . C27 . H272 . 109.4 no H271 . C27 . H272 . 109.5 no C25 . C27 . H273 . 110.6 no H271 . C27 . H273 . 109.5 no H272 . C27 . H273 . 109.5 no C10 . C28 . C29 . 111.2(18) yes C10 . C28 . C30 . 111.1(18) yes C29 . C28 . C30 . 107.6(18) yes C10 . C28 . H281 . 106.0 no C29 . C28 . H281 . 110.8 no C30 . C28 . H281 . 110.1 no C28 . C29 . H291 . 109.3 no C28 . C29 . H292 . 109.2 no H291 . C29 . H292 . 109.5 no C28 . C29 . H293 . 109.9 no H291 . C29 . H293 . 109.5 no H292 . C29 . H293 . 109.5 no C28 . C30 . H301 . 109.5 no C28 . C30 . H302 . 109.9 no H301 . C30 . H302 . 109.5 no C28 . C30 . H303 . 109.1 no H301 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no C12 . C31 . C32 . 117.4(16) yes C12 . C31 . C33 . 107.9(16) yes C32 . C31 . C33 . 109.9(17) yes C12 . C31 . H311 . 103.5 no C32 . C31 . H311 . 104.0 no C33 . C31 . H311 . 114.2 no C31 . C32 . H321 . 108.8 no C31 . C32 . H322 . 109.2 no H321 . C32 . H322 . 109.5 no C31 . C32 . H323 . 110.3 no H321 . C32 . H323 . 109.5 no H322 . C32 . H323 . 109.5 no C31 . C33 . H331 . 108.9 no C31 . C33 . H332 . 111.0 no H331 . C33 . H332 . 109.5 no C31 . C33 . H333 . 108.5 no H331 . C33 . H333 . 109.5 no H332 . C33 . H333 . 109.5 no C16 . C34 . C35 . 110.8(17) yes C16 . C34 . C36 . 107.1(18) yes C35 . C34 . C36 . 112.4(18) yes C16 . C34 . H341 . 112.2 no C35 . C34 . H341 . 105.4 no C36 . C34 . H341 . 108.9 no C34 . C35 . H351 . 109.9 no C34 . C35 . H352 . 108.7 no H351 . C35 . H352 . 109.5 no C34 . C35 . H353 . 109.8 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no C34 . C36 . H361 . 110.1 no C34 . C36 . H362 . 109.3 no H361 . C36 . H362 . 109.5 no C34 . C36 . H363 . 109.0 no H361 . C36 . H363 . 109.5 no H362 . C36 . H363 . 109.5 no O3 . Li1 . Cl2 . 121.4(19) yes O3 . Li1 . Cl1 . 110.7(18) yes Cl2 . Li1 . Cl1 . 95.9(15) yes O3 . Li1 . O2 . 108(2) yes Cl2 . Li1 . O2 . 111.3(18) yes Cl1 . Li1 . O2 . 108.3(18) yes #============================================== data_[tBuNON]UI3Li(THF)2 _database_code_depnum_ccdc_archive 'CCDC 271010' #============================================================= # CHEMICAL DATA _chemical_formula_sum ' C20 H46 I3 Li1 N2 O3 Si2 U1 ' _chemical_formula_moiety ' C20 H46 I3 Li1 N2 O3 Si2 U1 ' _chemical_formula_weight 1044.45 _chemical_absolute_configuration unk #============================================================= # CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y,z+1/2 #--------------------------------------------------------------- _cell_length_a 11.259(3) _cell_angle_alpha 90 _cell_length_b 13.222(4) _cell_angle_beta 92.45(2) _cell_length_c 12.012(3) _cell_angle_gamma 90 _cell_volume 1786.5(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 32 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _cell_measurement_temperature 293 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' green ' _exptl_crystal_size_min 0.09 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.36 _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 6.959 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.2539 _exptl_absorpt_correction_T_max 0.3236 #============================================================= # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.709 _diffrn_measurement_device_type 'Enraf-Nonius CAD4F' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w/2\q _diffrn_ambient_temperature 293 _diffrn_reflns_number 3335 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_theta_min 2.287 _diffrn_reflns_theta_max 24.996 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.996 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_interval_time 100 _diffrn_standards_interval_count 28 _diffrn_standards_number 2 _diffrn_standards_decay_% 1.41 #============================================================= # REFINEMENT DATA # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 3294 _reflns_threshold_expression I>2.50u(I) _reflns_number_gt 1673 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_gt 0.0380 _refine_ls_number_reflns 1673 _refine_ls_number_restraints 2 _refine_ls_number_parameters 188 #_refine_ls_R_factor_ref 0.0337 _refine_ls_wR_factor_ref 0.0380 _refine_ls_goodness_of_fit_ref 1.0276 _refine_ls_abs_structure_Flack 0.023(17) _refine_ls_abs_structure_details 'Flack, 0 Friedel-pairs' _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo) + (0.025Fo)^2^] ; _refine_ls_shift/su_max 0.001620 _refine_diff_density_min -0.46 _refine_diff_density_max 0.77 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min -14 _reflns_limit_l_max 14 #_reflns_number_all 3294 _refine_ls_R_factor_all 0.1241 _refine_ls_wR_factor_all 0.0468 # Number of reflections with Friedels Law is 3296 # Number of reflections without Friedels Law is 3294 # Theoretical number of reflections is about 3136 #--------------------------------------------------------------- _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; Ortep-3 (Farrugia 1997) ; #============================================================= # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'U ' -10.6730 9.6540 36.0228 0.5293 23.4128 3.3253 14.9491 16.0927 4.1880 100.6130 13.3966 International_Tables_Vol_IV_Table_2.2B 'I ' -0.7260 1.8120 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8777 4.0712 International_Tables_Vol_IV_Table_2.2B 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6938 1.1407 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'Li ' 0.0000 0.0000 1.1282 3.9546 0.7508 1.0524 0.6175 85.3906 0.4653 168.2610 0.0377 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B #============================================================= _computing_data_collection ; NRC DIFRAC ; _computing_data_reduction ; NRC DIFRAC ; _computing_cell_refinement ; NRC DIFRAC ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; #============================================================= # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_disorder_assembly _atom_site_refinement_disorder_group _atom_site_attached_hydrogens U1 U 0.6976(3) 0.24808(9) 0.0176(3) 0.0517 1.0000 Uani . . . . . . I1 I 0.5912(3) 0.07013(16) -0.1314(3) 0.0906 1.0000 Uani . . . . . . I2 I 0.6633(3) 0.09986(15) 0.2161(3) 0.0817 1.0000 Uani . . . . . . I3 I 0.7200(4) 0.38570(19) -0.1830(3) 0.1067 1.0000 Uani . . . . . . Si1 Si 0.6494(8) 0.4265(5) 0.1798(7) 0.0734 1.0000 Uani . . . . . . Si2 Si 0.9193(6) 0.3465(5) 0.1418(6) 0.0646 1.0000 Uani . . . . . . N1 N 0.5701(16) 0.3519(14) 0.0875(14) 0.0618 1.0000 Uani . . . . . . N2 N 0.8911(14) 0.2523(14) 0.0480(13) 0.0605 1.0000 Uani . . . . . . O1 O 0.7774(15) 0.3715(12) 0.1589(15) 0.0780 1.0000 Uani . . . . . . O2 O 0.7381(16) -0.1430(14) 0.0537(17) 0.1024 1.0000 Uani . . . . . . O3 O 0.4612(17) -0.1082(12) 0.0828(17) 0.1043 1.0000 Uani . . . . . . C1 C 0.665(3) 0.562(2) 0.145(3) 0.143(13) 1.0000 Uiso . . . . . . C2 C 0.619(3) 0.410(2) 0.330(2) 0.111(10) 1.0000 Uiso . . . . . . C3 C 0.989(3) 0.4555(19) 0.086(2) 0.096(9) 1.0000 Uiso . . . . . . C4 C 0.989(3) 0.314(2) 0.274(2) 0.122(11) 1.0000 Uiso . . . . . . C5 C 0.435(3) 0.358(2) 0.061(3) 0.103(10) 1.0000 Uiso . . . . . . C6 C 0.402(4) 0.291(3) -0.029(4) 0.181(17) 1.0000 Uiso . . . . . . C7 C 0.372(3) 0.328(2) 0.159(3) 0.133(12) 1.0000 Uiso . . . . . . C8 C 0.402(4) 0.465(3) 0.039(3) 0.183(18) 1.0000 Uiso . . . . . . C9 C 0.981(2) 0.192(2) -0.010(2) 0.071(7) 1.0000 Uiso . . . . . . C10 C 0.924(3) 0.116(2) -0.083(2) 0.113(11) 1.0000 Uiso . . . . . . C11 C 1.068(3) 0.141(3) 0.074(3) 0.143(13) 1.0000 Uiso . . . . . . C12 C 1.057(3) 0.253(2) -0.081(3) 0.125(11) 1.0000 Uiso . . . . . . C13 C 0.774(3) -0.185(3) -0.047(3) 0.124(11) 1.0000 Uiso . . . . . . C14 C 0.896(4) -0.229(3) -0.014(3) 0.175(17) 1.0000 Uiso . . . . . . C15 C 0.915(4) -0.215(3) 0.099(3) 0.145(13) 1.0000 Uiso . . . . . . C16 C 0.814(3) -0.166(2) 0.144(3) 0.119(11) 1.0000 Uiso . . . . . . C17 C 0.356(3) -0.054(3) 0.080(3) 0.133(12) 1.0000 Uiso . . . . . . C18 C 0.251(3) -0.121(2) 0.061(3) 0.119(11) 1.0000 Uiso . . . . . . C19 C 0.304(3) -0.215(2) 0.035(3) 0.121(11) 1.0000 Uiso . . . . . . C20 C 0.430(3) -0.207(2) 0.081(2) 0.100(9) 1.0000 Uiso . . . . . . Li1 Li 0.607(6) -0.056(4) 0.066(5) 0.116(18) 1.0000 Uiso . . . . . . H11 H 0.682 0.567 0.068 0.17(3) 1.0000 Uiso R . . . . . H12 H 0.727 0.593 0.188 0.17(3) 1.0000 Uiso R . . . . . H13 H 0.592 0.596 0.157 0.17(3) 1.0000 Uiso R . . . . . H21 H 0.613 0.341 0.348 0.11(3) 1.0000 Uiso R . . . . . H22 H 0.681 0.441 0.375 0.11(3) 1.0000 Uiso R . . . . . H23 H 0.546 0.443 0.343 0.11(3) 1.0000 Uiso R . . . . . H31 H 0.951 0.4722 0.016 0.08(3) 1.0000 Uiso R . . . . . H32 H 1.070 0.4411 0.076 0.08(3) 1.0000 Uiso R . . . . . H33 H 0.982 0.5108 0.136 0.08(3) 1.0000 Uiso R . . . . . H41 H 0.950 0.256 0.301 0.13(3) 1.0000 Uiso R . . . . . H42 H 1.071 0.298 0.266 0.13(3) 1.0000 Uiso R . . . . . H43 H 0.983 0.368 0.326 0.13(3) 1.0000 Uiso R . . . . . H61 H 0.318 0.299 -0.043 0.17(2) 1.0000 Uiso R . . . . . H62 H 0.442 0.309 -0.095 0.17(2) 1.0000 Uiso R . . . . . H63 H 0.419 0.222 -0.011 0.17(2) 1.0000 Uiso R . . . . . H71 H 0.289 0.332 0.143 0.11(2) 1.0000 Uiso R . . . . . H72 H 0.393 0.373 0.219 0.11(2) 1.0000 Uiso R . . . . . H73 H 0.393 0.261 0.180 0.11(2) 1.0000 Uiso R . . . . . H81 H 0.319 0.469 0.021 0.19(2) 1.0000 Uiso R . . . . . H82 H 0.421 0.507 0.102 0.19(2) 1.0000 Uiso R . . . . . H83 H 0.445 0.488 -0.023 0.19(2) 1.0000 Uiso R . . . . . H101 H 0.984 0.079 -0.119 0.11(2) 1.0000 Uiso R . . . . . H102 H 0.871 0.145 -0.137 0.11(2) 1.0000 Uiso R . . . . . H103 H 0.881 0.071 -0.038 0.11(2) 1.0000 Uiso R . . . . . H111 H 1.125 0.102 0.037 0.14(2) 1.0000 Uiso R . . . . . H112 H 1.108 0.191 0.118 0.14(2) 1.0000 Uiso R . . . . . H113 H 1.025 0.098 0.121 0.14(2) 1.0000 Uiso R . . . . . H121 H 1.112 0.211 -0.118 0.11(2) 1.0000 Uiso R . . . . . H122 H 1.099 0.300 -0.035 0.11(2) 1.0000 Uiso R . . . . . H123 H 1.009 0.288 -0.136 0.11(2) 1.0000 Uiso R . . . . . H131 H 0.779 -0.137 -0.106 0.16(3) 1.0000 Uiso R . . . . . H132 H 0.719 -0.237 -0.070 0.16(3) 1.0000 Uiso R . . . . . H141 H 0.955 -0.198 -0.057 0.21(3) 1.0000 Uiso R . . . . . H142 H 0.896 -0.300 -0.027 0.21(3) 1.0000 Uiso R . . . . . H151 H 0.979 -0.168 0.107 0.18(3) 1.0000 Uiso R . . . . . H152 H 0.936 -0.276 0.137 0.18(3) 1.0000 Uiso R . . . . . H161 H 0.835 -0.109 0.189 0.15(3) 1.0000 Uiso R . . . . . H162 H 0.776 -0.215 0.189 0.15(3) 1.0000 Uiso R . . . . . H171 H 0.348 -0.020 0.149 0.17(3) 1.0000 Uiso R . . . . . H172 H 0.358 -0.005 0.022 0.17(3) 1.0000 Uiso R . . . . . H181 H 0.205 -0.125 0.125 0.15(3) 1.0000 Uiso R . . . . . H182 H 0.202 -0.097 0.000 0.15(3) 1.0000 Uiso R . . . . . H191 H 0.262 -0.268 0.069 0.15(3) 1.0000 Uiso R . . . . . H192 H 0.304 -0.225 -0.044 0.15(3) 1.0000 Uiso R . . . . . H201 H 0.481 -0.245 0.036 0.13(3) 1.0000 Uiso R . . . . . H202 H 0.434 -0.234 0.154 0.13(3) 1.0000 Uiso 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 U1 0.0419(3) 0.0619(4) 0.0509(4) 0.0009(4) -0.0007(3) 0.0013(5) I1 0.0990(16) 0.0999(14) 0.0710(11) -0.0136(12) -0.0182(10) -0.0170(13) I2 0.112(2) 0.0718(12) 0.0612(13) 0.0083(10) 0.0048(13) -0.0097(13) I3 0.109(2) 0.129(2) 0.0825(16) 0.0446(14) 0.0054(15) 0.0134(16) Si1 0.066(5) 0.062(4) 0.093(5) -0.010(4) 0.008(4) 0.007(4) Si2 0.048(4) 0.087(5) 0.058(4) 0.005(4) -0.003(3) -0.010(4) N1 0.042(11) 0.084(13) 0.059(11) 0.002(10) 0.003(9) 0.016(10) N2 0.048(9) 0.068(11) 0.066(11) 0.013(11) 0.008(8) 0.028(12) O1 0.064(12) 0.070(11) 0.100(13) -0.014(10) -0.006(10) -0.019(10) O2 0.079(14) 0.107(14) 0.118(15) -0.015(12) -0.020(12) 0.025(11) O3 0.071(13) 0.057(11) 0.183(19) -0.003(11) -0.004(13) 0.007(9) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag U1 . O1 . 2.494(16) yes U1 . N2 . 2.194(16) yes U1 . N1 . 2.179(17) yes U1 . I3 . 3.039(3) yes U1 . I2 . 3.123(2) yes U1 . I1 . 3.161(2) yes I1 . Li1 . 2.90(6) yes I2 . Li1 . 2.79(6) yes Si1 . C2 . 1.86(3) yes Si1 . C1 . 1.85(3) yes Si1 . O1 . 1.643(19) yes Si1 . N1 . 1.707(19) yes Si2 . C4 . 1.80(3) yes Si2 . C3 . 1.78(3) yes Si2 . O1 . 1.654(19) yes Si2 . N2 . 1.701(19) yes N1 . C5 . 1.55(4) yes N2 . C9 . 1.49(3) yes O2 . Li1 . 1.88(6) yes O2 . C16 . 1.39(3) yes O2 . C13 . 1.41(3) yes O3 . Li1 . 1.80(6) yes O3 . C20 . 1.36(3) yes O3 . C17 . 1.39(4) yes C1 . H13 . 0.950 no C1 . H12 . 0.950 no C1 . H11 . 0.950 no C2 . H23 . 0.950 no C2 . H22 . 0.950 no C2 . H21 . 0.950 no C3 . H33 . 0.950 no C3 . H32 . 0.950 no C3 . H31 . 0.950 no C4 . H43 . 0.950 no C4 . H42 . 0.950 no C4 . H41 . 0.950 no C5 . C8 . 1.48(4) yes C5 . C7 . 1.45(4) yes C5 . C6 . 1.44(5) yes C6 . H63 . 0.950 no C6 . H62 . 0.950 no C6 . H61 . 0.950 no C7 . H73 . 0.950 no C7 . H72 . 0.950 no C7 . H71 . 0.950 no C8 . H83 . 0.950 no C8 . H82 . 0.950 no C8 . H81 . 0.950 no C9 . C12 . 1.47(4) yes C9 . C11 . 1.54(4) yes C9 . C10 . 1.47(4) yes C10 . H103 . 0.950 no C10 . H102 . 0.950 no C10 . H101 . 0.950 no C11 . H113 . 0.950 no C11 . H112 . 0.950 no C11 . H111 . 0.950 no C12 . H123 . 0.950 no C12 . H122 . 0.950 no C12 . H121 . 0.950 no C13 . H132 . 0.950 no C13 . H131 . 0.950 no C13 . C14 . 1.54(5) yes C14 . H142 . 0.950 no C14 . H141 . 0.950 no C14 . C15 . 1.38(5) yes C15 . H152 . 0.950 no C15 . H151 . 0.950 no C15 . C16 . 1.43(4) yes C16 . H162 . 0.950 no C16 . H161 . 0.950 no C17 . H172 . 0.950 no C17 . H171 . 0.950 no C17 . C18 . 1.49(4) yes C18 . H182 . 0.950 no C18 . H181 . 0.950 no C18 . C19 . 1.43(4) yes C19 . H192 . 0.950 no C19 . H191 . 0.950 no C19 . C20 . 1.50(4) yes C20 . H202 . 0.950 no C20 . H201 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . U1 . N2 . 62.9(6) yes O1 . U1 . N1 . 63.2(6) yes N2 . U1 . N1 . 125.8(7) yes O1 . U1 . I3 . 96.2(4) yes N2 . U1 . I3 . 90.1(4) yes N1 . U1 . I3 . 90.4(5) yes O1 . U1 . I2 . 86.8(4) yes N2 . U1 . I2 . 92.5(4) yes N1 . U1 . I2 . 89.8(5) yes I3 . U1 . I2 . 176.74(9) yes O1 . U1 . I1 . 171.6(4) yes N2 . U1 . I1 . 117.5(5) yes N1 . U1 . I1 . 116.6(5) yes I3 . U1 . I1 . 92.23(8) yes I2 . U1 . I1 . 84.79(6) yes Li1 . I1 . U1 . 87.4(11) yes Li1 . I2 . U1 . 90.1(12) yes C2 . Si1 . C1 . 110.8(14) yes C2 . Si1 . O1 . 107.2(13) yes C1 . Si1 . O1 . 107.5(14) yes C2 . Si1 . N1 . 116.8(12) yes C1 . Si1 . N1 . 117.6(13) yes O1 . Si1 . N1 . 94.7(9) yes C4 . Si2 . C3 . 110.2(14) yes C4 . Si2 . O1 . 109.1(13) yes C3 . Si2 . O1 . 109.0(12) yes C4 . Si2 . N2 . 118.2(12) yes C3 . Si2 . N2 . 114.5(10) yes O1 . Si2 . N2 . 94.3(8) yes C5 . N1 . U1 . 128.0(18) yes C5 . N1 . Si1 . 125.8(18) yes U1 . N1 . Si1 . 106.3(9) yes C9 . N2 . U1 . 126.8(15) yes C9 . N2 . Si2 . 126.3(15) yes U1 . N2 . Si2 . 106.6(8) yes Si1 . O1 . Si2 . 165.1(11) yes Si1 . O1 . U1 . 95.8(7) yes Si2 . O1 . U1 . 96.1(8) yes Li1 . O2 . C16 . 122(3) yes Li1 . O2 . C13 . 124(3) yes C16 . O2 . C13 . 114(2) yes Li1 . O3 . C20 . 127(3) yes Li1 . O3 . C17 . 125(2) yes C20 . O3 . C17 . 106(2) yes H13 . C1 . H12 . 109.476 no H13 . C1 . H11 . 109.476 no H12 . C1 . H11 . 109.476 no H13 . C1 . Si1 . 109.068 no H12 . C1 . Si1 . 111.357 no H11 . C1 . Si1 . 107.956 no H23 . C2 . H22 . 109.476 no H23 . C2 . H21 . 109.475 no H22 . C2 . H21 . 109.476 no H23 . C2 . Si1 . 107.687 no H22 . C2 . Si1 . 110.008 no H21 . C2 . Si1 . 110.689 no H33 . C3 . H32 . 109.476 no H33 . C3 . H31 . 109.475 no H32 . C3 . H31 . 109.476 no H33 . C3 . Si2 . 109.749 no H32 . C3 . Si2 . 109.099 no H31 . C3 . Si2 . 109.552 no H43 . C4 . H42 . 109.476 no H43 . C4 . H41 . 109.476 no H42 . C4 . H41 . 109.476 no H43 . C4 . Si2 . 110.538 no H42 . C4 . Si2 . 110.248 no H41 . C4 . Si2 . 107.597 no C8 . C5 . C7 . 106(3) yes C8 . C5 . C6 . 114(3) yes C7 . C5 . C6 . 109(3) yes C8 . C5 . N1 . 109(3) yes C7 . C5 . N1 . 109(3) yes C6 . C5 . N1 . 110(3) yes H63 . C6 . H62 . 109.476 no H63 . C6 . H61 . 109.476 no H62 . C6 . H61 . 109.476 no H63 . C6 . C5 . 111.542 no H62 . C6 . C5 . 110.395 no H61 . C6 . C5 . 106.416 no H73 . C7 . H72 . 109.476 no H73 . C7 . H71 . 109.476 no H72 . C7 . H71 . 109.476 no H73 . C7 . C5 . 110.167 no H72 . C7 . C5 . 109.257 no H71 . C7 . C5 . 108.973 no H83 . C8 . H82 . 109.476 no H83 . C8 . H81 . 109.476 no H82 . C8 . H81 . 109.476 no H83 . C8 . C5 . 107.706 no H82 . C8 . C5 . 111.398 no H81 . C8 . C5 . 109.275 no C12 . C9 . C11 . 105(3) yes C12 . C9 . C10 . 106(2) yes C11 . C9 . C10 . 110(2) yes C12 . C9 . N2 . 113(2) yes C11 . C9 . N2 . 111(2) yes C10 . C9 . N2 . 111(2) yes H103 . C10 . H102 . 109.476 no H103 . C10 . H101 . 109.476 no H102 . C10 . H101 . 109.476 no H103 . C10 . C9 . 108.228 no H102 . C10 . C9 . 111.697 no H101 . C10 . C9 . 108.453 no H113 . C11 . H112 . 109.476 no H113 . C11 . H111 . 109.476 no H112 . C11 . H111 . 109.476 no H113 . C11 . C9 . 108.861 no H112 . C11 . C9 . 108.895 no H111 . C11 . C9 . 110.638 no H123 . C12 . H122 . 109.476 no H123 . C12 . H121 . 109.476 no H122 . C12 . H121 . 109.476 no H123 . C12 . C9 . 109.885 no H122 . C12 . C9 . 108.099 no H121 . C12 . C9 . 110.407 no H132 . C13 . H131 . 109.467 no H132 . C13 . C14 . 111.021 no H131 . C13 . C14 . 111.489 no H132 . C13 . O2 . 108.986 no H131 . C13 . O2 . 113.439 no C14 . C13 . O2 . 102(3) yes H142 . C14 . H141 . 109.467 no H142 . C14 . C15 . 107.117 no H141 . C14 . C15 . 113.291 no H142 . C14 . C13 . 109.858 no H141 . C14 . C13 . 109.494 no C15 . C14 . C13 . 108(4) yes H152 . C15 . H151 . 109.467 no H152 . C15 . C16 . 112.860 no H151 . C15 . C16 . 106.278 no H152 . C15 . C14 . 111.911 no H151 . C15 . C14 . 105.812 no C16 . C15 . C14 . 110(4) yes H162 . C16 . H161 . 109.467 no H162 . C16 . O2 . 108.231 no H161 . C16 . O2 . 113.005 no H162 . C16 . C15 . 107.009 no H161 . C16 . C15 . 112.921 no O2 . C16 . C15 . 106(3) yes H172 . C17 . H171 . 109.467 no H172 . C17 . C18 . 109.473 no H171 . C17 . C18 . 108.265 no H172 . C17 . O3 . 108.590 no H171 . C17 . O3 . 109.397 no C18 . C17 . O3 . 112(3) yes H182 . C18 . H181 . 109.467 no H182 . C18 . C19 . 110.666 no H181 . C18 . C19 . 111.875 no H182 . C18 . C17 . 110.722 no H181 . C18 . C17 . 111.701 no C19 . C18 . C17 . 102(3) yes H192 . C19 . H191 . 109.467 no H192 . C19 . C20 . 110.048 no H191 . C19 . C20 . 111.691 no H192 . C19 . C18 . 111.098 no H191 . C19 . C18 . 109.294 no C20 . C19 . C18 . 105(3) yes H202 . C20 . H201 . 109.467 no H202 . C20 . O3 . 109.674 no H201 . C20 . O3 . 110.336 no H202 . C20 . C19 . 109.059 no H201 . C20 . C19 . 110.070 no O3 . C20 . C19 . 108(3) yes O3 . Li1 . O2 . 120(3) yes O3 . Li1 . I1 . 107(3) yes O2 . Li1 . I1 . 108(3) yes O3 . Li1 . I2 . 113(3) yes O2 . Li1 . I2 . 110(3) yes I1 . Li1 . I2 . 96.3(17) yes #========================================================================== data_{[Me3PhNON]ThCl3Li(THF)2}2 _database_code_depnum_ccdc_archive 'CCDC 271011' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= # CHEMICAL DATA _chemical_formula_sum ' C14.50 H24.5 Cl1.50 Li0.50 N1 O1 Si1 Th0.50 ' _chemical_formula_moiety ' C14.50 H24.5 Cl1.50 Li0.50 N1 O1 Si1 Th0.50 ' _chemical_formula_weight 429.6 #========================================================================== # CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z x,-y,z -x+1/2,y+1/2,-z x+1/2,-y+1/2,z #-------------------------------------------------------------------------- _cell_length_a 24.157(5) _cell_angle_alpha 90 _cell_length_b 17.397(4) _cell_angle_beta 99.17(2) _cell_length_c 9.239(2) _cell_angle_gamma 90 _cell_volume 3833.2(15) _cell_formula_units_Z 8 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 293 #-------------------------------------------------------------------------- _exptl_crystal_description ' block ' _exptl_crystal_colour ' colorless ' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.45 _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1678.876 _exptl_absorpt_coefficient_mu 14.6407 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _empir_absorpt_correction_T_min 0.0083 _empir_absorpt_correction_T_max 1.0000 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 # Number of reflections with Friedels Law is 3531 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3510 #========================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w/2\q _diffrn_ambient_temperature 293 _diffrn_reflns_number 3531 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_theta_min 3.144 _diffrn_reflns_theta_max 68.245 _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 51.866 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_radiation_monochromator graphite #============================================================= # REFINEMENT DATA # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 3531 _reflns_number_gt 2355 _reflns_threshold_expression I>3.00u(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.0597 _refine_ls_number_reflns 2355 _refine_ls_number_parameters 190 _refine_ls_number_restraints 19 _refine_ls_goodness_of_fit_ref 1.0002 _refine_ls_weighting_scheme calc #_reflns_number_all 3513 _refine_ls_R_factor_all 0.0761 _refine_ls_wR_factor_all 0.0873 #_refine_ls_R_factor_ref 0.0469 _refine_ls_wR_factor_gt 0.0597 _refine_ls_weighting_details ; w=1/[\s^2^(Fo) + (0.026Fo)^2^] ; _refine_ls_shift/su_max 0.000111 _refine_diff_density_max 1.84 _refine_diff_density_min -1.12 _reflns_limit_h_min -29 _reflns_limit_h_max 28 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 10 _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; # Uequiv = arithmetic mean of Ui loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Th ' -4.1491 12.3296 35.5645 0.5634 23.4219 3.4620 12.7473 17.8309 4.8070 99.1722 13.4314 International_Tables_Vol_IV_Table_2.2B 'Si ' 0.2541 0.3302 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'C ' 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Li ' 0.0008 0.0003 1.1282 3.9546 0.7508 1.0524 0.6175 85.3905 0.4653 168.2610 0.0377 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B #============================================================= 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Th1 Th 0.10172(2) 0.0000 0.05042(7) 0.0430 1.0000 Uani S T . . . . Cl1 Cl 0.0851(2) 0.0000 -0.2496(5) 0.0846 1.0000 Uani S T . . . . Cl2 Cl 0.0000 -0.0971(2) 0.0000 0.0727 1.0000 Uani S T . . . . Cl3 Cl 0.0779(2) 0.0000 0.3273(5) 0.0718 1.0000 Uani S T . . . . Si1 Si 0.21546(14) 0.0917(2) 0.0057(4) 0.0651 1.0000 Uani . . . . . . O1 O 0.2022(5) 0.0000 -0.0334(14) 0.0700 1.0000 Uani S T . . . . O2 O 0.0108(8) -0.1586(15) -0.396(2) 0.1033 0.5000 Uani D . . . 1 . N1 N 0.1567(4) 0.1075(5) 0.0896(10) 0.0538 1.0000 Uani . . . . . . C1 C 0.2175(7) 0.1428(12) -0.1662(17) 0.1086 1.0000 Uani . . . . . . C2 C 0.2844(6) 0.1053(11) 0.1283(19) 0.1011 1.0000 Uani . . . . . . C3 C 0.1518(5) 0.1791(7) 0.1635(14) 0.0627 1.0000 Uani . . . . . . C4 C 0.1247(5) 0.2428(7) 0.0953(16) 0.0685 1.0000 Uani . . . . . . C5 C 0.1219(6) 0.3105(8) 0.176(2) 0.0888 1.0000 Uani . . . . . . C6 C 0.1439(6) 0.3167(9) 0.320(2) 0.0820 1.0000 Uani . . . . . . C7 C 0.1704(6) 0.2539(9) 0.3909(19) 0.0825 1.0000 Uani . . . . . . C8 C 0.1741(5) 0.1850(8) 0.3160(15) 0.0657 1.0000 Uani . . . . . . C9 C 0.0987(6) 0.2391(9) -0.0669(16) 0.0860 1.0000 Uani . . . . . . C10 C 0.1389(10) 0.3934(10) 0.399(3) 0.1505 1.0000 Uani . . . . . . C11 C 0.2022(7) 0.1183(10) 0.4024(15) 0.0904 1.0000 Uani . . . . . . C12 C 0.459(2) 0.000000(7) 0.280(6) 0.33(2) 1.0000 Uiso DS . . . . . C13 C 0.4541(17) 0.000000(10) 0.112(5) 0.33(2) 1.0000 Uiso DS . . . . . C14 C 0.5026(9) 0.000000(10) 0.075(4) 0.33(2) 1.0000 Uiso DS . . . . . C16 C -0.0359(18) -0.198(3) -0.427(6) 0.133(16) 0.5000 Uiso D . . . 1 . C17 C -0.0326(17) -0.255(3) -0.549(4) 0.129(14) 0.5000 Uiso D . . . 1 . C18 C 0.0156(18) -0.230(3) -0.606(4) 0.110(13) 0.5000 Uiso D . . . 1 . C19 C 0.0492(12) -0.184(2) -0.478(4) 0.091(9) 0.5000 Uiso D . . . 1 . Li1 Li 0.0045(17) -0.071(3) -0.291(4) 0.063(10) 0.5000 Uiso . . . . . . H11 H 0.2251 0.1956 -0.1461 0.16(3) 1.0000 Uiso R . . . . . H12 H 0.2464 0.1215 -0.2127 0.16(3) 1.0000 Uiso R . . . . . H13 H 0.1825 0.1379 -0.2291 0.16(3) 1.0000 Uiso R . . . . . H21 H 0.2906 0.1585 0.1482 0.14(3) 1.0000 Uiso R . . . . . H22 H 0.3134 0.0857 0.0807 0.14(3) 1.0000 Uiso R . . . . . H23 H 0.2841 0.0785 0.2178 0.14(3) 1.0000 Uiso R . . . . . H51 H 0.1043 0.3542 0.1268 0.15(6) 1.0000 Uiso R . . . . . H71 H 0.1862 0.2575 0.4917 0.14(6) 1.0000 Uiso R . . . . . H91 H 0.0932 0.1870 -0.0965 0.12(2) 1.0000 Uiso R . . . . . H92 H 0.1235 0.2632 -0.1230 0.12(2) 1.0000 Uiso R . . . . . H93 H 0.0637 0.2652 -0.0817 0.12(2) 1.0000 Uiso R . . . . . H101 H 0.1707 0.4245 0.3926 0.20(2) 0.5000 Uiso R . . . . . H102 H 0.1369 0.3838 0.4997 0.20(2) 0.5000 Uiso R . . . . . H103 H 0.1059 0.4198 0.3558 0.20(2) 0.5000 Uiso R . . . . . H104 H 0.1050 0.3943 0.4394 0.20(2) 0.5000 Uiso R . . . . . H105 H 0.1698 0.3990 0.4762 0.20(2) 0.5000 Uiso R . . . . . H106 H 0.1388 0.4349 0.3324 0.20(2) 0.5000 Uiso R . . . . . H111 H 0.2184 0.0811 0.3465 0.13(2) 1.0000 Uiso R . . . . . H112 H 0.2312 0.1377 0.4749 0.13(2) 1.0000 Uiso R . . . . . H113 H 0.1749 0.0931 0.4487 0.13(2) 1.0000 Uiso R . . . . . H121 H 0.4246 0.0000 0.3191 0.36(2) 1.0000 Uiso RS . . . . . H122 H 0.4798 -0.0446 0.3122 0.36(2) 1.0000 Uiso R . . . . . H131 H 0.4330 -0.0446 0.0800 0.36(2) 1.0000 Uiso R . . . . . H141 H 0.5210 -0.0446 0.1183 0.36(2) 1.0000 Uiso R . . . . . H161 H -0.0652 -0.1624 -0.4574 0.17(5) 0.5000 Uiso R . . 1 1 . H162 H -0.0439 -0.2257 -0.3438 0.17(5) 0.5000 Uiso R . . 1 1 . H171 H -0.0646 -0.2507 -0.6236 0.17(5) 0.5000 Uiso R . . 1 1 . H172 H -0.0292 -0.3059 -0.5138 0.17(5) 0.5000 Uiso R . . 1 1 . H181 H 0.0365 -0.2738 -0.6287 0.14(5) 0.5000 Uiso R . . 1 1 . H182 H 0.0066 -0.1990 -0.6904 0.14(5) 0.5000 Uiso R . . 1 1 . H191 H 0.0766 -0.2153 -0.4215 0.12(5) 0.5000 Uiso R . . 1 1 . H192 H 0.0671 -0.1405 -0.5136 0.12(5) 0.5000 Uiso R . . 1 1 . 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 Th1 0.0351(3) 0.0423(3) 0.0531(4) 0.0000 0.0113(2) 0.0000 Cl1 0.070(3) 0.119(5) 0.066(3) 0.0000 0.015(2) 0.0000 Cl2 0.049(2) 0.0406(19) 0.128(4) 0.0000 0.011(2) 0.0000 Cl3 0.071(3) 0.091(3) 0.055(3) 0.0000 0.016(2) 0.0000 Si1 0.0515(16) 0.0611(19) 0.086(2) 0.0058(19) 0.0207(16) -0.0109(16) O1 0.054(6) 0.067(7) 0.083(8) 0.0000 -0.004(6) 0.0000 O2 0.083(13) 0.12(2) 0.122(15) -0.066(15) 0.062(12) -0.016(13) N1 0.057(5) 0.046(5) 0.060(6) 0.005(5) 0.016(4) -0.007(4) C1 0.106(12) 0.123(15) 0.108(12) 0.029(12) 0.052(10) -0.013(12) C2 0.059(8) 0.113(14) 0.129(13) -0.010(12) 0.006(9) -0.020(9) C3 0.062(7) 0.050(6) 0.076(9) -0.003(6) 0.014(6) -0.006(6) C4 0.055(6) 0.045(6) 0.106(11) 0.006(7) 0.015(7) -0.004(5) C5 0.060(8) 0.053(7) 0.156(16) 0.009(10) 0.024(10) 0.002(7) C6 0.068(8) 0.067(9) 0.112(12) -0.018(9) 0.017(8) -0.010(7) C7 0.062(8) 0.074(9) 0.112(12) -0.022(9) 0.016(8) -0.013(7) C8 0.058(7) 0.063(7) 0.076(9) -0.008(7) 0.008(6) -0.011(6) C9 0.064(8) 0.069(9) 0.119(13) 0.029(9) -0.003(8) -0.012(7) C10 0.155(19) 0.066(10) 0.23(2) -0.062(15) 0.033(18) 0.002(12) C11 0.112(12) 0.087(11) 0.066(9) 0.016(8) -0.005(8) -0.015(10) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.04152(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Th1 . N1 6_555 2.289(9) yes Th1 . Cl2 6_555 2.957(2) yes Th1 . Cl1 . 2.737(5) yes Th1 . Cl2 . 2.957(2) yes Th1 . Cl3 . 2.710(5) yes Th1 . O1 . 2.664(13) yes Th1 . N1 . 2.289(9) yes Cl1 . Li1 6_555 2.29(4) yes Cl1 . Li1 . 2.29(4) yes Cl2 . Li1 5_555 2.74(4) yes Cl2 . Li1 . 2.74(4) yes Cl3 . Li1 2_555 2.32(4) yes Cl3 . Li1 5_555 2.32(4) yes Si1 . O1 . 1.656(5) yes Si1 . N1 . 1.743(10) yes Si1 . C1 . 1.828(15) yes Si1 . C2 . 1.873(14) yes O2 . C16 . 1.31(4) yes O2 . C19 . 1.35(3) yes O2 . Li1 . 1.83(5) yes N1 . C3 . 1.435(15) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . H21 . 0.950 no C2 . H22 . 0.950 no C2 . H23 . 0.950 no C3 . C4 . 1.386(17) yes C3 . C8 . 1.429(18) yes C4 . C5 . 1.40(2) yes C4 . C9 . 1.531(19) yes C5 . C6 . 1.36(2) yes C5 . H51 . 0.950 no C6 . C7 . 1.38(2) yes C6 . C10 . 1.54(2) yes C7 . C8 . 1.394(19) yes C7 . H71 . 0.950 no C8 . C11 . 1.508(19) yes C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no C10 . H101 . 0.950 no C10 . H102 . 0.950 no C10 . H103 . 0.950 no C10 . H104 . 0.950 no C10 . H105 . 0.950 no C10 . H106 . 0.950 no C11 . H111 . 0.950 no C11 . H112 . 0.950 no C11 . H113 . 0.950 no C12 . H122 6_555 0.950 no C12 . C13 . 1.54(5) yes C12 . H121 . 0.950 no C12 . H122 . 0.950 no C13 . H131 6_555 0.950 no C13 . C14 . 1.27(6) yes C13 . H131 . 0.950 no C14 . C14 2_655 1.38(7) yes C14 . H141 6_555 0.950 no C14 . H141 . 0.950 no C16 . C17 . 1.51(5) yes C16 . H161 . 0.950 no C16 . H162 . 0.950 no C17 . C18 . 1.41(4) yes C17 . H171 . 0.950 no C17 . H172 . 0.950 no C18 . C19 . 1.56(4) yes C18 . H181 . 0.950 no C18 . H182 . 0.950 no C19 . H191 . 0.950 no C19 . H192 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 6_555 Th1 . Cl2 6_555 159.8(3) yes N1 6_555 Th1 . Cl1 . 98.5(2) yes Cl2 6_555 Th1 . Cl1 . 81.72(9) yes N1 6_555 Th1 . Cl2 . 90.3(2) yes Cl2 6_555 Th1 . Cl2 . 69.65(13) yes Cl1 . Th1 . Cl2 . 81.72(9) yes N1 6_555 Th1 . Cl3 . 93.2(2) yes Cl2 6_555 Th1 . Cl3 . 81.50(8) yes Cl1 . Th1 . Cl3 . 159.52(15) yes Cl2 . Th1 . Cl3 . 81.50(8) yes N1 6_555 Th1 . O1 . 60.9(3) yes Cl2 6_555 Th1 . O1 . 136.67(15) yes Cl1 . Th1 . O1 . 72.5(3) yes Cl2 . Th1 . O1 . 136.67(15) yes Cl3 . Th1 . O1 . 128.0(3) yes N1 6_555 Th1 . N1 . 109.5(5) yes Cl2 6_555 Th1 . N1 . 90.3(2) yes Cl1 . Th1 . N1 . 98.5(2) yes Cl2 . Th1 . N1 . 159.8(3) yes Cl3 . Th1 . N1 . 93.2(2) yes O1 . Th1 . N1 . 60.9(3) yes Th1 . Cl1 . Li1 6_555 98.7(10) yes Th1 . Cl1 . Li1 . 98.7(10) yes Li1 6_555 Cl1 . Li1 . 66(2) yes Th1 . Cl2 . Th1 2_555 110.35(13) yes Th1 . Cl2 . Li1 5_555 85.1(9) yes Th1 2_555 Cl2 . Li1 5_555 84.2(9) yes Th1 . Cl2 . Li1 . 84.2(9) yes Th1 2_555 Cl2 . Li1 . 85.1(9) yes Li1 5_555 Cl2 . Li1 . 161.2(19) yes Th1 . Cl3 . Li1 2_555 99.7(10) yes Th1 . Cl3 . Li1 5_555 99.7(10) yes Li1 2_555 Cl3 . Li1 5_555 65(2) yes O1 . Si1 . N1 . 96.1(6) yes O1 . Si1 . C1 . 108.0(8) yes N1 . Si1 . C1 . 116.5(7) yes O1 . Si1 . C2 . 112.1(7) yes N1 . Si1 . C2 . 114.8(7) yes C1 . Si1 . C2 . 108.6(8) yes Th1 . O1 . Si1 . 95.1(5) yes Th1 . O1 . Si1 6_555 95.1(5) yes Si1 . O1 . Si1 6_555 149.0(8) yes C16 . O2 . C19 . 111(2) yes C16 . O2 . Li1 . 114(2) yes C19 . O2 . Li1 . 133(2) yes Th1 . N1 . Si1 . 107.1(5) yes Th1 . N1 . C3 . 134.0(8) yes Si1 . N1 . C3 . 118.9(8) yes Si1 . C1 . H11 . 109.4 no Si1 . C1 . H12 . 109.0 no H11 . C1 . H12 . 109.5 no Si1 . C1 . H13 . 110.0 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no Si1 . C2 . H21 . 109.8 no Si1 . C2 . H22 . 109.0 no H21 . C2 . H22 . 109.5 no Si1 . C2 . H23 . 109.6 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no N1 . C3 . C4 . 123.2(11) yes N1 . C3 . C8 . 119.0(11) yes C4 . C3 . C8 . 117.8(12) yes C3 . C4 . C5 . 119.4(14) yes C3 . C4 . C9 . 120.1(12) yes C5 . C4 . C9 . 120.5(13) yes C4 . C5 . C6 . 122.9(14) yes C4 . C5 . H51 . 118.5 no C6 . C5 . H51 . 118.6 no C5 . C6 . C7 . 118.9(15) yes C5 . C6 . C10 . 119.3(17) yes C7 . C6 . C10 . 121.8(16) yes C6 . C7 . C8 . 120.4(15) yes C6 . C7 . H71 . 119.8 no C8 . C7 . H71 . 119.8 no C3 . C8 . C7 . 120.5(13) yes C3 . C8 . C11 . 122.2(12) yes C7 . C8 . C11 . 117.2(12) yes C4 . C9 . H91 . 109.8 no C4 . C9 . H92 . 108.6 no H91 . C9 . H92 . 109.6 no C4 . C9 . H93 . 109.8 no H91 . C9 . H93 . 109.6 no H92 . C9 . H93 . 109.5 no C6 . C10 . H101 . 109.6 no C6 . C10 . H102 . 109.5 no H101 . C10 . H102 . 109.3 no C6 . C10 . H103 . 109.9 no H101 . C10 . H103 . 109.3 no H102 . C10 . H103 . 109.3 no C6 . C10 . H104 . 109.7 no H101 . C10 . H104 . 140.7 no H102 . C10 . H104 . 56.2 no H103 . C10 . H104 . 56.2 no C6 . C10 . H105 . 109.4 no H101 . C10 . H105 . 56.2 no H102 . C10 . H105 . 56.2 no H103 . C10 . H105 . 140.7 no H104 . C10 . H105 . 109.3 no C6 . C10 . H106 . 109.9 no H101 . C10 . H106 . 56.2 no H102 . C10 . H106 . 140.7 no H103 . C10 . H106 . 56.2 no H104 . C10 . H106 . 109.3 no H105 . C10 . H106 . 109.3 no C8 . C11 . H111 . 115.3 no C8 . C11 . H112 . 108.5 no H111 . C11 . H112 . 107.8 no C8 . C11 . H113 . 107.9 no H111 . C11 . H113 . 107.8 no H112 . C11 . H113 . 109.5 no H122 6_555 C12 . C13 . 105.4 no H122 6_555 C12 . H121 . 109.5 no C13 . C12 . H121 . 117.3 no H122 6_555 C12 . H122 . 109.5 no C13 . C12 . H122 . 105.4 no H121 . C12 . H122 . 109.5 no C12 . C13 . H131 6_555 105.2 no C12 . C13 . C14 . 110.5(10) yes H131 6_555 C13 . C14 . 113.0 no C12 . C13 . H131 . 105.2 no H131 6_555 C13 . H131 . 109.5 no C14 . C13 . H131 . 113.0 no C14 2_655 C14 . H141 6_555 112.5 no C14 2_655 C14 . C13 . 109.4(10) yes H141 6_555 C14 . C13 . 106.2 no C14 2_655 C14 . H141 . 112.5 no H141 6_555 C14 . H141 . 109.5 no C13 . C14 . H141 . 106.2 no O2 . C16 . C17 . 111(2) yes O2 . C16 . H161 . 107.2 no C17 . C16 . H161 . 109.0 no O2 . C16 . H162 . 111.8 no C17 . C16 . H162 . 108.5 no H161 . C16 . H162 . 109.5 no C16 . C17 . C18 . 103(2) yes C16 . C17 . H171 . 111.2 no C18 . C17 . H171 . 109.4 no C16 . C17 . H172 . 111.4 no C18 . C17 . H172 . 112.0 no H171 . C17 . H172 . 109.5 no C17 . C18 . C19 . 104(2) yes C17 . C18 . H181 . 110.2 no C19 . C18 . H181 . 110.7 no C17 . C18 . H182 . 112.4 no C19 . C18 . H182 . 110.3 no H181 . C18 . H182 . 109.5 no C18 . C19 . O2 . 106(2) yes C18 . C19 . H191 . 110.2 no O2 . C19 . H191 . 111.1 no C18 . C19 . H192 . 111.1 no O2 . C19 . H192 . 109.3 no H191 . C19 . H192 . 109.5 no Cl3 5_555 Li1 . Cl1 . 114.8(19) yes Cl3 5_555 Li1 . Cl2 . 93.6(14) yes Cl1 . Li1 . Cl2 . 95.3(13) yes Cl3 5_555 Li1 . O2 . 121(2) yes Cl1 . Li1 . O2 . 113(2) yes Cl2 . Li1 . O2 . 114(2) yes #============================================================= data_[ipr2PhNCOCN]U(CH2SiMe3)2 _database_code_depnum_ccdc_archive 'CCDC 271012' #============================================================= # CHEMICAL DATA _chemical_formula_sum ' C36 H64 N2 O1 Si2 U1 ' _chemical_formula_moiety ' C36 H64 N2 O1 Si2 U1 ' _chemical_formula_weight 835.12 #============================================================= # CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 #-------------------------------------------------------------- _cell_length_a 11.4344(13) _cell_length_b 20.450(5) _cell_length_c 35.450(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8289(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 293 _exptl_crystal_description ' orange ' _exptl_crystal_colour ' plate ' _exptl_crystal_size_min 0.09 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_max 0.75 _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_meas ? _exptl_crystal_F_000 3376 _exptl_absorpt_coefficient_mu 3.794 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.00 _exptl_absorpt_correction_T_max 0.00 # Number of reflections with Friedels Law is 7203 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7270 #============================================================= # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.70930 _diffrn_measurement_device_type 'Enraf Nonius CAD4F' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w/2\q _diffrn_ambient_temperature 293 _diffrn_reflns_number 7345 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_theta_min 1.988 _diffrn_reflns_theta_max 24.997 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 24.497 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 42 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 #============================================================= # REFINEMENT DATA # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 7203 _reflns_number_gt 2613 _reflns_threshold_expression I>2.50u(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.0686 _refine_ls_number_reflns 2613 _refine_ls_number_restraints 0 _refine_ls_number_parameters 316 _refine_ls_goodness_of_fit_ref 1.6350 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo) + (0.03Fo)^2^] ; _refine_ls_shift/su_max 0.017073 _refine_diff_density_min ? _refine_diff_density_max ? _reflns_limit_h_min 0 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 42 #_reflns_number_all 7203 _refine_ls_R_factor_all 0.2200 _refine_ls_wR_factor_all 0.0817 #-------------------------------------------------------------------- _chemical_name_systematic # IUPAC name, in full ; ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; Ortep-3 (Farrugia 1997) ; #============================================================= # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'U ' -10.6730 9.6540 36.0228 0.5293 23.4128 3.3253 14.9491 16.0927 4.1880 100.6130 13.3966 International_Tables_Vol_IV_Table_2.2B 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6938 1.1407 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B #============================================================= _computing_data_collection ; NRC DIFRAc ; _computing_data_reduction ; NRC DIFRAC ; _computing_cell_refinement ; NRC DIFRAC ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; #============================================================= # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_disorder_assembly _atom_site_refinement_disorder_group _atom_site_attached_hydrogens U1 U 0.44078(6) 0.34993(4) 0.13171(2) 0.0438 1.0000 Uani . . . . . . Si1 Si 0.4352(7) 0.3099(4) 0.2377(2) 0.0846 1.0000 Uani . . . . . . Si2 Si 0.7554(6) 0.3860(3) 0.1002(2) 0.0599 1.0000 Uani . . . . . . O1 O 0.2243(10) 0.3268(6) 0.1393(5) 0.0707 1.0000 Uani . . . . . . N1 N 0.3340(14) 0.4411(8) 0.1382(4) 0.0420 1.0000 Uani . . . . . . N2 N 0.3880(12) 0.2478(9) 0.1145(4) 0.0428 1.0000 Uani . . . . . . C1 C 0.2105(19) 0.4425(11) 0.1478(7) 0.0709 1.0000 Uani . . . . . . C2 C 0.1490(19) 0.3814(11) 0.1338(9) 0.0888 1.0000 Uani . . . . . . C3 C 0.1844(17) 0.2661(10) 0.1228(6) 0.0616 1.0000 Uani . . . . . . C4 C 0.2781(17) 0.2174(11) 0.1245(7) 0.0660 1.0000 Uani . . . . . . C5 C 0.3841(18) 0.5039(9) 0.1286(8) 0.0572 1.0000 Uani . . . . . . C6 C 0.444(2) 0.5425(11) 0.1523(8) 0.0662 1.0000 Uani . . . . . . C7 C 0.504(2) 0.5986(13) 0.1407(7) 0.0739 1.0000 Uani . . . . . . C8 C 0.501(2) 0.6164(13) 0.1014(9) 0.0825 1.0000 Uani . . . . . . C9 C 0.436(3) 0.5814(13) 0.0803(10) 0.0968 1.0000 Uani . . . . . . C10 C 0.378(2) 0.5254(12) 0.0883(7) 0.0636 1.0000 Uani . . . . . . C11 C 0.4701(17) 0.2083(10) 0.0951(7) 0.0522 1.0000 Uani . . . . . . C12 C 0.547(2) 0.1629(10) 0.1137(7) 0.0585 1.0000 Uani . . . . . . C13 C 0.626(2) 0.1275(12) 0.0937(11) 0.1020 1.0000 Uani . . . . . . C14 C 0.620(3) 0.1262(14) 0.0524(9) 0.0927 1.0000 Uani . . . . . . C15 C 0.551(2) 0.1707(11) 0.0337(8) 0.0801 1.0000 Uani . . . . . . C16 C 0.4713(16) 0.2119(9) 0.0554(7) 0.0520 1.0000 Uani . . . . . . C17 C 0.443(2) 0.5251(12) 0.1943(7) 0.0725 1.0000 Uani . . . . . . C18 C 0.302(2) 0.4879(14) 0.0615(8) 0.0917 1.0000 Uani . . . . . . C19 C 0.544(2) 0.1567(10) 0.1566(6) 0.0580 1.0000 Uani . . . . . . C20 C 0.392(2) 0.2583(13) 0.0348(7) 0.0788 1.0000 Uani . . . . . . C21 C 0.559(2) 0.5342(12) 0.2147(8) 0.105(9) 1.0000 Uiso . . . . . . C22 C 0.345(2) 0.5665(14) 0.2146(8) 0.119(11) 1.0000 Uiso . . . . . . C23 C 0.359(2) 0.4770(14) 0.0231(9) 0.121(12) 1.0000 Uiso . . . . . . C24 C 0.185(3) 0.5200(14) 0.0533(9) 0.133(12) 1.0000 Uiso . . . . . . C25 C 0.667(2) 0.1543(12) 0.1743(7) 0.090(8) 1.0000 Uiso . . . . . . C26 C 0.479(2) 0.0924(12) 0.1670(8) 0.085(9) 1.0000 Uiso . . . . . . C27 C 0.444(2) 0.2911(12) -0.0020(8) 0.102(9) 1.0000 Uiso . . . . . . C28 C 0.279(3) 0.2202(14) 0.0214(9) 0.131(12) 1.0000 Uiso . . . . . . C29 C 0.5142(17) 0.3318(11) 0.1941(6) 0.0575 1.0000 Uani . . . . . . C30 C 0.5985(16) 0.3810(11) 0.0890(6) 0.0626 1.0000 Uani . . . . . . C31 C 0.352(3) 0.2325(15) 0.2315(9) 0.142(13) 1.0000 Uiso . . . . . . C32 C 0.328(3) 0.3731(13) 0.2497(10) 0.146(13) 1.0000 Uiso . . . . . . C33 C 0.523(4) 0.287(2) 0.2787(12) 0.22(2) 1.0000 Uiso . . . . . . C34 C 0.813(3) 0.3013(15) 0.1084(10) 0.149(14) 1.0000 Uiso . . . . . . C35 C 0.779(3) 0.4367(15) 0.1408(8) 0.124(12) 1.0000 Uiso . . . . . . C36 C 0.846(2) 0.4269(12) 0.0621(7) 0.093(9) 1.0000 Uiso . . . . . . H11 H 0.2028 0.4426 0.1745 0.04(2) 1.0000 Uiso R . . . . . H12 H 0.1759 0.4810 0.1377 0.04(2) 1.0000 Uiso R . . . . . H21 H 0.0757 0.3746 0.1458 0.06(2) 1.0000 Uiso R . . . . . H22 H 0.1374 0.3868 0.1075 0.06(2) 1.0000 Uiso R . . . . . H31 H 0.1169 0.2511 0.1359 0.03(2) 1.0000 Uiso R . . . . . H32 H 0.1655 0.2732 0.0971 0.03(2) 1.0000 Uiso R . . . . . H41 H 0.2831 0.2015 0.1496 0.04(2) 1.0000 Uiso R . . . . . H42 H 0.2623 0.1821 0.1079 0.04(2) 1.0000 Uiso R . . . . . H71 H 0.545 0.6251 0.1584 0.07(3) 1.0000 Uiso R . . . . . H81 H 0.546 0.6517 0.0917 0.08(3) 1.0000 Uiso R . . . . . H91 H 0.426 0.5971 0.0553 0.10(3) 1.0000 Uiso R . . . . . H131 H 0.684 0.1025 0.1064 0.10(3) 1.0000 Uiso R . . . . . H141 H 0.665 0.0952 0.0386 0.09(3) 1.0000 Uiso R . . . . . H151 H 0.555 0.1750 0.0070 0.08(3) 1.0000 Uiso R . . . . . H171 H 0.426 0.4799 0.1968 0.10(5) 1.0000 Uiso R . . . . . H181 H 0.292 0.4459 0.0725 0.12(5) 1.0000 Uiso R . . . . . H191 H 0.504 0.1940 0.1661 0.08(5) 1.0000 Uiso R . . . . . H201 H 0.380 0.2939 0.0516 0.10(5) 1.0000 Uiso R . . . . . H211 H 0.553 0.5219 0.2405 0.115(19) 1.0000 Uiso R . . . . . H212 H 0.579 0.5791 0.2130 0.115(19) 1.0000 Uiso R . . . . . H213 H 0.617 0.5086 0.2026 0.115(19) 1.0000 Uiso R . . . . . H221 H 0.340 0.5569 0.2408 0.124(19) 1.0000 Uiso R . . . . . H222 H 0.367 0.6111 0.2114 0.124(19) 1.0000 Uiso R . . . . . H223 H 0.271 0.5589 0.2031 0.124(19) 1.0000 Uiso R . . . . . H231 H 0.310 0.4513 0.0073 0.130(19) 1.0000 Uiso R . . . . . H232 H 0.370 0.5189 0.0121 0.130(19) 1.0000 Uiso R . . . . . H233 H 0.432 0.4560 0.0259 0.130(19) 1.0000 Uiso R . . . . . H241 H 0.137 0.4953 0.0367 0.131(19) 1.0000 Uiso R . . . . . H242 H 0.201 0.5616 0.0425 0.131(19) 1.0000 Uiso R . . . . . H243 H 0.146 0.5255 0.0767 0.131(19) 1.0000 Uiso R . . . . . H251 H 0.662 0.1519 0.2010 0.106(19) 1.0000 Uiso R . . . . . H252 H 0.710 0.1919 0.1672 0.106(19) 1.0000 Uiso R . . . . . H253 H 0.704 0.1162 0.1649 0.106(19) 1.0000 Uiso R . . . . . H261 H 0.473 0.0889 0.1936 0.094(19) 1.0000 Uiso R . . . . . H262 H 0.523 0.0565 0.1574 0.094(19) 1.0000 Uiso R . . . . . H263 H 0.403 0.0922 0.1561 0.094(19) 1.0000 Uiso R . . . . . H271 H 0.387 0.3200 -0.0124 0.109(19) 1.0000 Uiso R . . . . . H272 H 0.513 0.3149 0.0040 0.109(19) 1.0000 Uiso R . . . . . H273 H 0.462 0.2580 -0.0199 0.109(19) 1.0000 Uiso R . . . . . H281 H 0.226 0.2484 0.0084 0.136(19) 1.0000 Uiso R . . . . . H282 H 0.242 0.2041 0.0436 0.136(19) 1.0000 Uiso R . . . . . H283 H 0.299 0.1845 0.0055 0.136(19) 1.0000 Uiso R . . . . . H291 H 0.5531 0.3714 0.2004 0.05(3) 1.0000 Uiso R . . . . . H292 H 0.5701 0.2978 0.1913 0.05(3) 1.0000 Uiso R . . . . . H301 H 0.5782 0.4234 0.0803 0.06(3) 1.0000 Uiso R . . . . . H302 H 0.5939 0.3508 0.0687 0.06(3) 1.0000 Uiso R . . . . . H311 H 0.311 0.2234 0.2544 0.20(3) 1.0000 Uiso R . . . . . H312 H 0.403 0.1974 0.2259 0.20(3) 1.0000 Uiso R . . . . . H313 H 0.297 0.2373 0.2116 0.20(3) 1.0000 Uiso R . . . . . H321 H 0.287 0.3608 0.2719 0.19(3) 1.0000 Uiso R . . . . . H322 H 0.367 0.4135 0.2538 0.19(3) 1.0000 Uiso R . . . . . H323 H 0.274 0.3777 0.2294 0.19(3) 1.0000 Uiso R . . . . . H331 H 0.470 0.277 0.2988 0.28(3) 1.0000 Uiso R . . . . . H332 H 0.573 0.322 0.2861 0.28(3) 1.0000 Uiso R . . . . . H333 H 0.568 0.249 0.2729 0.28(3) 1.0000 Uiso R . . . . . H341 H 0.894 0.3023 0.1147 0.21(3) 1.0000 Uiso R . . . . . H342 H 0.771 0.2810 0.1283 0.21(3) 1.0000 Uiso R . . . . . H343 H 0.802 0.2771 0.0858 0.21(3) 1.0000 Uiso R . . . . . H351 H 0.860 0.4388 0.1467 0.16(3) 1.0000 Uiso R . . . . . H352 H 0.751 0.4794 0.1354 0.16(3) 1.0000 Uiso R . . . . . H353 H 0.737 0.4192 0.1617 0.16(3) 1.0000 Uiso R . . . . . H361 H 0.926 0.4278 0.0700 0.14(3) 1.0000 Uiso R . . . . . H362 H 0.819 0.4703 0.0580 0.14(3) 1.0000 Uiso R . . . . . H363 H 0.840 0.4027 0.0393 0.14(3) 1.0000 Uiso 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 U1 0.0336(3) 0.0437(4) 0.0540(5) -0.0037(6) -0.0019(5) -0.0012(5) Si1 0.066(4) 0.136(7) 0.052(5) -0.001(5) -0.004(4) 0.005(5) Si2 0.049(3) 0.059(5) 0.072(5) -0.004(4) 0.006(4) -0.003(3) O1 0.024(6) 0.043(8) 0.145(18) -0.015(10) 0.002(9) -0.006(6) N1 0.058(10) 0.061(11) 0.007(11) 0.000(9) 0.012(8) 0.008(9) N2 0.036(7) 0.047(10) 0.045(11) 0.002(9) -0.007(8) 0.016(9) C1 0.078(17) 0.043(14) 0.09(2) -0.008(14) 0.002(14) 0.000(14) C2 0.051(14) 0.071(16) 0.14(3) 0.01(2) 0.022(19) 0.023(13) C3 0.046(12) 0.088(19) 0.051(19) -0.017(14) 0.008(11) -0.002(13) C4 0.055(14) 0.070(15) 0.07(2) -0.016(15) -0.012(13) -0.013(13) C5 0.056(12) 0.033(12) 0.082(19) -0.009(15) -0.020(15) 0.004(11) C6 0.053(12) 0.048(13) 0.10(2) -0.003(14) -0.015(16) -0.011(14) C7 0.074(15) 0.084(19) 0.06(2) -0.024(16) -0.014(14) -0.017(15) C8 0.081(18) 0.066(18) 0.10(3) 0.037(19) 0.009(18) -0.011(16) C9 0.09(2) 0.068(19) 0.14(3) 0.01(2) 0.02(2) 0.00(2) C10 0.080(17) 0.062(17) 0.049(17) 0.004(14) -0.003(14) -0.004(15) C11 0.057(15) 0.042(12) 0.057(18) -0.010(13) -0.012(12) 0.001(11) C12 0.046(13) 0.035(14) 0.094(18) -0.012(13) -0.010(13) -0.012(12) C13 0.070(17) 0.064(18) 0.17(4) -0.01(2) 0.04(2) 0.032(14) C14 0.11(2) 0.09(2) 0.07(2) 0.002(19) 0.033(19) 0.030(18) C15 0.10(2) 0.069(16) 0.070(19) -0.001(14) 0.027(18) 0.014(17) C16 0.048(13) 0.035(11) 0.073(19) -0.001(13) 0.005(12) 0.009(10) C17 0.074(15) 0.075(17) 0.069(18) -0.032(14) -0.026(17) -0.004(17) C18 0.11(2) 0.10(2) 0.07(2) 0.034(19) 0.011(18) 0.018(19) C19 0.084(17) 0.036(12) 0.054(15) -0.016(14) -0.023(14) 0.013(16) C20 0.088(18) 0.085(19) 0.063(18) 0.010(17) -0.010(14) 0.002(16) C29 0.043(11) 0.068(17) 0.062(17) 0.009(13) -0.009(11) 0.009(11) C30 0.061(14) 0.060(14) 0.067(17) -0.015(13) -0.016(13) 0.002(12) _refine_ls_extinction_coef 26(18) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag U1 . C30 . 2.44(2) yes U1 . C29 . 2.40(2) yes U1 . N2 . 2.257(18) yes U1 . N1 . 2.241(16) yes U1 . O1 . 2.535(12) yes Si1 . C33 . 1.83(4) yes Si1 . C32 . 1.83(3) yes Si1 . C31 . 1.86(3) yes Si1 . C29 . 1.84(2) yes Si2 . C36 . 1.90(2) yes Si2 . C35 . 1.79(3) yes Si2 . C34 . 1.88(3) yes Si2 . C30 . 1.841(19) yes O1 . C3 . 1.45(2) yes O1 . C2 . 1.42(2) yes N1 . C5 . 1.45(2) yes N1 . C1 . 1.45(2) yes N2 . C11 . 1.42(2) yes N2 . C4 . 1.45(2) yes C1 . H12 . 0.950 no C1 . H11 . 0.950 no C1 . C2 . 1.52(3) yes C2 . H22 . 0.950 no C2 . H21 . 0.950 no C3 . H32 . 0.950 no C3 . H31 . 0.950 no C3 . C4 . 1.46(3) yes C4 . H42 . 0.950 no C4 . H41 . 0.950 no C5 . C10 . 1.50(3) yes C5 . C6 . 1.34(3) yes C6 . C17 . 1.53(3) yes C6 . C7 . 1.40(3) yes C7 . H71 . 0.950 no C7 . C8 . 1.44(4) yes C8 . H81 . 0.950 no C8 . C9 . 1.27(3) yes C9 . H91 . 0.950 no C9 . C10 . 1.35(3) yes C10 . C18 . 1.50(3) yes C11 . C16 . 1.41(3) yes C11 . C12 . 1.44(3) yes C12 . C19 . 1.53(3) yes C12 . C13 . 1.35(3) yes C13 . H131 . 0.950 no C13 . C14 . 1.46(4) yes C14 . H141 . 0.950 no C14 . C15 . 1.38(3) yes C15 . H151 . 0.950 no C15 . C16 . 1.46(3) yes C16 . C20 . 1.50(3) yes C17 . H171 . 0.950 no C17 . C22 . 1.58(3) yes C17 . C21 . 1.52(3) yes C18 . H181 . 0.950 no C18 . C24 . 1.52(3) yes C18 . C23 . 1.52(3) yes C19 . H191 . 0.950 no C19 . C26 . 1.55(3) yes C19 . C25 . 1.54(3) yes C20 . H201 . 0.950 no C20 . C28 . 1.59(3) yes C20 . C27 . 1.58(3) yes C21 . H213 . 0.950 no C21 . H212 . 0.950 no C21 . H211 . 0.950 no C22 . H223 . 0.950 no C22 . H222 . 0.950 no C22 . H221 . 0.950 no C23 . H233 . 0.950 no C23 . H232 . 0.950 no C23 . H231 . 0.950 no C24 . H243 . 0.950 no C24 . H242 . 0.950 no C24 . H241 . 0.950 no C25 . H253 . 0.950 no C25 . H252 . 0.950 no C25 . H251 . 0.950 no C26 . H263 . 0.950 no C26 . H262 . 0.950 no C26 . H261 . 0.950 no C27 . H273 . 0.950 no C27 . H272 . 0.950 no C27 . H271 . 0.950 no C28 . H283 . 0.950 no C28 . H282 . 0.950 no C28 . H281 . 0.950 no C29 . H292 . 0.950 no C29 . H291 . 0.950 no C30 . H302 . 0.950 no C30 . H301 . 0.950 no C31 . H313 . 0.950 no C31 . H312 . 0.950 no C31 . H311 . 0.950 no C32 . H323 . 0.950 no C32 . H322 . 0.950 no C32 . H321 . 0.950 no C33 . H333 . 0.950 no C33 . H332 . 0.950 no C33 . H331 . 0.950 no C34 . H343 . 0.950 no C34 . H342 . 0.950 no C34 . H341 . 0.950 no C35 . H353 . 0.950 no C35 . H352 . 0.950 no C35 . H351 . 0.950 no C36 . H363 . 0.950 no C36 . H362 . 0.950 no C36 . H361 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C30 . U1 . C29 . 110.8(6) yes C30 . U1 . N2 . 105.7(7) yes C29 . U1 . N2 . 101.6(7) yes C30 . U1 . N1 . 104.5(6) yes C29 . U1 . N1 . 103.0(6) yes N2 . U1 . N1 . 130.6(5) yes C30 . U1 . O1 . 146.8(6) yes C29 . U1 . O1 . 102.4(6) yes N2 . U1 . O1 . 66.1(5) yes N1 . U1 . O1 . 67.2(5) yes C33 . Si1 . C32 . 111.3(18) yes C33 . Si1 . C31 . 99.0(17) yes C32 . Si1 . C31 . 106.4(13) yes C33 . Si1 . C29 . 117.4(16) yes C32 . Si1 . C29 . 110.6(13) yes C31 . Si1 . C29 . 111.1(13) yes C36 . Si2 . C35 . 103.6(13) yes C36 . Si2 . C34 . 109.0(14) yes C35 . Si2 . C34 . 110.9(15) yes C36 . Si2 . C30 . 113.8(12) yes C35 . Si2 . C30 . 110.5(12) yes C34 . Si2 . C30 . 108.9(13) yes C3 . O1 . C2 . 115.3(16) yes C3 . O1 . U1 . 115.2(11) yes C2 . O1 . U1 . 115.4(11) yes C5 . N1 . C1 . 115.0(17) yes C5 . N1 . U1 . 119.9(12) yes C1 . N1 . U1 . 124.8(14) yes C11 . N2 . C4 . 116.7(17) yes C11 . N2 . U1 . 118.8(12) yes C4 . N2 . U1 . 124.3(13) yes H12 . C1 . H11 . 109.467 no H12 . C1 . C2 . 111.543 no H11 . C1 . C2 . 106.528 no H12 . C1 . N1 . 109.388 no H11 . C1 . N1 . 108.916 no C2 . C1 . N1 . 110.9(18) yes H22 . C2 . H21 . 109.467 no H22 . C2 . O1 . 108.037 no H21 . C2 . O1 . 111.026 no H22 . C2 . C1 . 106.855 no H21 . C2 . C1 . 112.508 no O1 . C2 . C1 . 108.8(19) yes H32 . C3 . H31 . 109.467 no H32 . C3 . C4 . 107.972 no H31 . C3 . C4 . 110.882 no H32 . C3 . O1 . 109.236 no H31 . C3 . O1 . 109.603 no C4 . C3 . O1 . 109.6(16) yes H42 . C4 . H41 . 109.467 no H42 . C4 . N2 . 109.889 no H41 . C4 . N2 . 108.895 no H42 . C4 . C3 . 110.690 no H41 . C4 . C3 . 108.343 no N2 . C4 . C3 . 109.5(18) yes C10 . C5 . C6 . 117(2) yes C10 . C5 . N1 . 118(2) yes C6 . C5 . N1 . 125(2) yes C17 . C6 . C7 . 119(2) yes C17 . C6 . C5 . 118(2) yes C7 . C6 . C5 . 123(3) yes H71 . C7 . C8 . 120.405 no H71 . C7 . C6 . 120.887 no C8 . C7 . C6 . 119(2) yes H81 . C8 . C9 . 121.843 no H81 . C8 . C7 . 121.993 no C9 . C8 . C7 . 116(3) yes H91 . C9 . C10 . 115.156 no H91 . C9 . C8 . 115.302 no C10 . C9 . C8 . 130(3) yes C18 . C10 . C9 . 126(3) yes C18 . C10 . C5 . 119(2) yes C9 . C10 . C5 . 115(3) yes C16 . C11 . C12 . 119(2) yes C16 . C11 . N2 . 117.4(19) yes C12 . C11 . N2 . 124(2) yes C19 . C12 . C13 . 120(3) yes C19 . C12 . C11 . 119(2) yes C13 . C12 . C11 . 121(3) yes H131 . C13 . C14 . 119.564 no H131 . C13 . C12 . 120.079 no C14 . C13 . C12 . 120(3) yes H141 . C14 . C15 . 120.069 no H141 . C14 . C13 . 120.266 no C15 . C14 . C13 . 120(3) yes H151 . C15 . C16 . 119.932 no H151 . C15 . C14 . 120.978 no C16 . C15 . C14 . 119(2) yes C20 . C16 . C11 . 120.8(20) yes C20 . C16 . C15 . 119(2) yes C11 . C16 . C15 . 120(2) yes H171 . C17 . C22 . 109.512 no H171 . C17 . C21 . 104.514 no C22 . C17 . C21 . 109.5(20) yes H171 . C17 . C6 . 108.591 no C22 . C17 . C6 . 109(2) yes C21 . C17 . C6 . 116(2) yes H181 . C18 . C24 . 111.116 no H181 . C18 . C23 . 106.784 no C24 . C18 . C23 . 105(2) yes H181 . C18 . C10 . 105.843 no C24 . C18 . C10 . 114(2) yes C23 . C18 . C10 . 113(2) yes H191 . C19 . C26 . 111.585 no H191 . C19 . C25 . 108.818 no C26 . C19 . C25 . 108.0(19) yes H191 . C19 . C12 . 107.423 no C26 . C19 . C12 . 108.6(18) yes C25 . C19 . C12 . 112(2) yes H201 . C20 . C28 . 116.513 no H201 . C20 . C27 . 104.345 no C28 . C20 . C27 . 106(2) yes H201 . C20 . C16 . 105.376 no C28 . C20 . C16 . 109(2) yes C27 . C20 . C16 . 116(2) yes H213 . C21 . H212 . 109.476 no H213 . C21 . H211 . 109.476 no H212 . C21 . H211 . 109.475 no H213 . C21 . C17 . 109.177 no H212 . C21 . C17 . 107.399 no H211 . C21 . C17 . 111.794 no H223 . C22 . H222 . 109.476 no H223 . C22 . H221 . 109.476 no H222 . C22 . H221 . 109.476 no H223 . C22 . C17 . 110.219 no H222 . C22 . C17 . 105.925 no H221 . C22 . C17 . 112.190 no H233 . C23 . H232 . 109.476 no H233 . C23 . H231 . 109.476 no H232 . C23 . H231 . 109.476 no H233 . C23 . C18 . 110.378 no H232 . C23 . C18 . 106.895 no H231 . C23 . C18 . 111.095 no H243 . C24 . H242 . 109.476 no H243 . C24 . H241 . 109.476 no H242 . C24 . H241 . 109.476 no H243 . C24 . C18 . 107.322 no H242 . C24 . C18 . 107.546 no H241 . C24 . C18 . 113.461 no H253 . C25 . H252 . 109.476 no H253 . C25 . H251 . 109.476 no H252 . C25 . H251 . 109.476 no H253 . C25 . C19 . 107.316 no H252 . C25 . C19 . 110.146 no H251 . C25 . C19 . 110.915 no H263 . C26 . H262 . 109.476 no H263 . C26 . H261 . 109.476 no H262 . C26 . H261 . 109.476 no H263 . C26 . C19 . 109.952 no H262 . C26 . C19 . 108.831 no H261 . C26 . C19 . 109.615 no H273 . C27 . H272 . 109.476 no H273 . C27 . H271 . 109.476 no H272 . C27 . H271 . 109.476 no H273 . C27 . C20 . 109.199 no H272 . C27 . C20 . 110.045 no H271 . C27 . C20 . 109.154 no H283 . C28 . H282 . 109.476 no H283 . C28 . H281 . 109.476 no H282 . C28 . H281 . 109.476 no H283 . C28 . C20 . 110.820 no H282 . C28 . C20 . 106.332 no H281 . C28 . C20 . 111.200 no H292 . C29 . H291 . 109.467 no H292 . C29 . U1 . 104.499 no H291 . C29 . U1 . 104.291 no H292 . C29 . Si1 . 103.985 no H291 . C29 . Si1 . 103.990 no U1 . C29 . Si1 . 129.7(10) yes H302 . C30 . H301 . 109.467 no H302 . C30 . U1 . 105.123 no H301 . C30 . U1 . 104.988 no H302 . C30 . Si2 . 104.721 no H301 . C30 . Si2 . 104.936 no U1 . C30 . Si2 . 127.0(11) yes H313 . C31 . H312 . 109.476 no H313 . C31 . H311 . 109.476 no H312 . C31 . H311 . 109.476 no H313 . C31 . Si1 . 109.713 no H312 . C31 . Si1 . 110.294 no H311 . C31 . Si1 . 108.386 no H323 . C32 . H322 . 109.476 no H323 . C32 . H321 . 109.476 no H322 . C32 . H321 . 109.476 no H323 . C32 . Si1 . 109.235 no H322 . C32 . Si1 . 109.538 no H321 . C32 . Si1 . 109.628 no H333 . C33 . H332 . 109.476 no H333 . C33 . H331 . 109.475 no H332 . C33 . H331 . 109.476 no H333 . C33 . Si1 . 109.380 no H332 . C33 . Si1 . 111.216 no H331 . C33 . Si1 . 107.786 no H343 . C34 . H342 . 109.476 no H343 . C34 . H341 . 109.476 no H342 . C34 . H341 . 109.476 no H343 . C34 . Si2 . 107.650 no H342 . C34 . Si2 . 109.842 no H341 . C34 . Si2 . 110.891 no H353 . C35 . H352 . 109.476 no H353 . C35 . H351 . 109.476 no H352 . C35 . H351 . 109.475 no H353 . C35 . Si2 . 109.489 no H352 . C35 . Si2 . 108.625 no H351 . C35 . Si2 . 110.281 no H363 . C36 . H362 . 109.476 no H363 . C36 . H361 . 109.475 no H362 . C36 . H361 . 109.476 no H363 . C36 . Si2 . 109.569 no H362 . C36 . Si2 . 110.021 no H361 . C36 . Si2 . 108.807 no #============================================================= data_[MesNON]2Th _database_code_depnum_ccdc_archive 'CCDC 271013' #============================================================= # # Please forward any questions concerning # this CIF to Dr. Gabriele Schatte # (gabriele.schatte@usask.ca). #============================================================= # CHEMICAL DATA _chemical_formula_moiety 'C44 H68 N4 O2 Si4 Th' _chemical_formula_sum 'C44 H68 N4 O2 Si4 Th' _chemical_formula_weight 1029.42 #============================================================= # Crystal Data _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' #-------------------------------------------------------------- _cell_length_a 11.01900(10) _cell_length_b 20.3090(2) _cell_length_c 21.6470(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.4250(4) _cell_angle_gamma 90.00 _cell_volume 4791.99(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13782 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 3.250 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4971 _exptl_absorpt_correction_T_max 0.5923 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================= # EXPERIMENTAL DATA _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'KappaCCD (BruKer AXS-Nonius, FR540C)' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 26791 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 30.02 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.711 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.113 _reflns_number_total 13945 _reflns_number_gt 10814 _reflns_threshold_expression >2sigma(I) _computing_structure_solution ; SIR-97 (A. Altomare, G. Cascarano et al.) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Cameron (WinGX v1.64-05), Ortep (SHELXTL-NT v6.14, Bruker AXS) ; _computing_publication_material 'WinGX v1.64-05 (L. J. Farrugia)' #============================================================= # REFINEMENT DATA _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^)+(0.0113P)^2^+6.6299P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13945 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0627 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 #============================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Th1 Th 0.634167(10) 0.282214(5) 0.132928(5) 0.02217(4) Uani 1 1 d . . . Si21 Si 0.37409(8) 0.21788(4) 0.16253(5) 0.02821(19) Uani 1 1 d . . . Si31 Si 0.61507(8) 0.13202(4) 0.18825(4) 0.02590(19) Uani 1 1 d . . . Si61 Si 0.63782(9) 0.32493(4) -0.01363(4) 0.0297(2) Uani 1 1 d . . . Si71 Si 0.66607(9) 0.43569(4) 0.09120(5) 0.0331(2) Uani 1 1 d . . . O11 O 0.49551(18) 0.17351(10) 0.15013(10) 0.0260(5) Uani 1 1 d . . . O21 O 0.6065(2) 0.37640(10) 0.04223(10) 0.0294(5) Uani 1 1 d . . . N11 N 0.4307(2) 0.29479(12) 0.15068(13) 0.0270(6) Uani 1 1 d . . . N41 N 0.7217(2) 0.19429(12) 0.19262(13) 0.0270(6) Uani 1 1 d . . . N51 N 0.6556(2) 0.25445(12) 0.03038(13) 0.0273(6) Uani 1 1 d . . . N81 N 0.7157(2) 0.38720(12) 0.15400(13) 0.0296(6) Uani 1 1 d . . . C11 C 0.3528(3) 0.35100(14) 0.15452(15) 0.0259(6) Uani 1 1 d . . . C12 C 0.2774(3) 0.37386(16) 0.10065(16) 0.0317(7) Uani 1 1 d . . . C13 C 0.1983(3) 0.42707(16) 0.10573(17) 0.0340(8) Uani 1 1 d . . . H13 H 0.1474 0.4419 0.0691 0.041 Uiso 1 1 calc . . . C14 C 0.1909(3) 0.45877(16) 0.16132(18) 0.0350(8) Uani 1 1 d . . . C15 C 0.2686(3) 0.43651(16) 0.21305(18) 0.0376(8) Uani 1 1 d . . . H15 H 0.2669 0.4582 0.2518 0.045 Uiso 1 1 calc . . . C16 C 0.3496(3) 0.38383(16) 0.21144(16) 0.0318(7) Uani 1 1 d . . . C17 C 0.2819(4) 0.3445(2) 0.03750(18) 0.0521(11) Uani 1 1 d . . . H17A H 0.2357 0.3031 0.0336 0.063 Uiso 1 1 calc R . . H17B H 0.3674 0.3359 0.0324 0.063 Uiso 1 1 calc R . . H17C H 0.2454 0.3753 0.0052 0.063 Uiso 1 1 calc R . . C18 C 0.1015(4) 0.51390(18) 0.1661(2) 0.0487(10) Uani 1 1 d . . . H18A H 0.0325 0.4975 0.1855 0.058 Uiso 1 1 calc R . . H18B H 0.0710 0.5307 0.1243 0.058 Uiso 1 1 calc R . . H18C H 0.1426 0.5495 0.1917 0.058 Uiso 1 1 calc R . . C19 C 0.4308(4) 0.3640(2) 0.27085(19) 0.0532(11) Uani 1 1 d . . . H19A H 0.4392 0.4011 0.3001 0.064 Uiso 1 1 calc R . . H19B H 0.5119 0.3515 0.2612 0.064 Uiso 1 1 calc R . . H19C H 0.3940 0.3265 0.2898 0.064 Uiso 1 1 calc R . . C21 C 0.2378(3) 0.19127(18) 0.1074(2) 0.0442(10) Uani 1 1 d . . . H21A H 0.2567 0.1931 0.0645 0.053 Uiso 1 1 calc R . . H21B H 0.1687 0.2206 0.1112 0.053 Uiso 1 1 calc R . . H21C H 0.2160 0.1461 0.1172 0.053 Uiso 1 1 calc R . . C22 C 0.3355(3) 0.20277(19) 0.24219(19) 0.0436(9) Uani 1 1 d . . . H22A H 0.3129 0.1564 0.2461 0.052 Uiso 1 1 calc R . . H22B H 0.2664 0.2309 0.2491 0.052 Uiso 1 1 calc R . . H22C H 0.4068 0.2131 0.2733 0.052 Uiso 1 1 calc R . . C31 C 0.6350(3) 0.06036(16) 0.13799(17) 0.0366(8) Uani 1 1 d . . . H31A H 0.5611 0.0329 0.1338 0.044 Uiso 1 1 calc R . . H31B H 0.7058 0.0344 0.1569 0.044 Uiso 1 1 calc R . . H31C H 0.6485 0.0757 0.0966 0.044 Uiso 1 1 calc R . . C32 C 0.5885(3) 0.10227(17) 0.26628(17) 0.0352(8) Uani 1 1 d . . . H32A H 0.5731 0.1399 0.2923 0.042 Uiso 1 1 calc R . . H32B H 0.6611 0.0783 0.2862 0.042 Uiso 1 1 calc R . . H32C H 0.5172 0.0728 0.2615 0.042 Uiso 1 1 calc R . . C41 C 0.8291(3) 0.19345(17) 0.23927(17) 0.0331(8) Uani 1 1 d . . . C42 C 0.8312(3) 0.23181(19) 0.29306(18) 0.0405(9) Uani 1 1 d . . . C43 C 0.9368(4) 0.2326(3) 0.3375(2) 0.0621(14) Uani 1 1 d . . . H43 H 0.9388 0.2593 0.3737 0.075 Uiso 1 1 calc . . . C44 C 1.0389(4) 0.1953(3) 0.3299(3) 0.0737(18) Uani 1 1 d . . . C45 C 1.0347(3) 0.1578(3) 0.2775(3) 0.0635(15) Uani 1 1 d . . . H45 H 1.1042 0.1318 0.2724 0.076 Uiso 1 1 calc . . . C46 C 0.9323(3) 0.15598(19) 0.2307(2) 0.0452(10) Uani 1 1 d . . . C47 C 0.7232(4) 0.27361(18) 0.30372(19) 0.0459(9) Uani 1 1 d . . . H47A H 0.7332 0.2878 0.3475 0.055 Uiso 1 1 calc R . . H47B H 0.6475 0.2479 0.2941 0.055 Uiso 1 1 calc R . . H47C H 0.7185 0.3124 0.2765 0.055 Uiso 1 1 calc R . . C48 C 1.1530(5) 0.1973(4) 0.3792(3) 0.123(3) Uani 1 1 d . . . H48A H 1.1974 0.1555 0.3789 0.148 Uiso 1 1 calc R . . H48B H 1.1286 0.2041 0.4205 0.148 Uiso 1 1 calc R . . H48C H 1.2063 0.2335 0.3699 0.148 Uiso 1 1 calc R . . C49 C 0.9352(3) 0.1138(2) 0.1743(2) 0.0576(12) Uani 1 1 d . . . H49A H 0.9127 0.0685 0.1836 0.069 Uiso 1 1 calc R . . H49B H 1.0180 0.1142 0.1629 0.069 Uiso 1 1 calc R . . H49C H 0.8768 0.1309 0.1395 0.069 Uiso 1 1 calc R . . C51 C 0.6727(3) 0.19027(15) 0.00481(16) 0.0287(7) Uani 1 1 d . . . C52 C 0.5717(3) 0.14924(16) -0.01567(16) 0.0337(7) Uani 1 1 d . . . C53 C 0.5916(4) 0.08493(17) -0.03534(18) 0.0420(9) Uani 1 1 d . . . H53 H 0.5227 0.0579 -0.0494 0.050 Uiso 1 1 calc . . . C54 C 0.7075(4) 0.05963(17) -0.03493(18) 0.0442(9) Uani 1 1 d . . . C55 C 0.8064(4) 0.10085(17) -0.01673(19) 0.0415(9) Uani 1 1 d . . . H55 H 0.8870 0.0846 -0.0176 0.050 Uiso 1 1 calc . . . C56 C 0.7919(3) 0.16557(16) 0.00294(17) 0.0353(8) Uani 1 1 d . . . C57 C 0.4414(3) 0.17192(19) -0.0159(2) 0.0472(10) Uani 1 1 d . . . H57A H 0.4081 0.1881 -0.0575 0.057 Uiso 1 1 calc R . . H57B H 0.4399 0.2074 0.0147 0.057 Uiso 1 1 calc R . . H57C H 0.3915 0.1350 -0.0048 0.057 Uiso 1 1 calc R . . C58 C 0.7276(5) -0.01155(18) -0.0519(2) 0.0615(13) Uani 1 1 d . . . H58A H 0.7089 -0.0403 -0.0181 0.074 Uiso 1 1 calc R . . H58B H 0.8133 -0.0178 -0.0578 0.074 Uiso 1 1 calc R . . H58C H 0.6736 -0.0226 -0.0906 0.074 Uiso 1 1 calc R . . C59 C 0.9051(3) 0.20685(18) 0.0218(2) 0.0496(11) Uani 1 1 d . . . H59A H 0.9781 0.1814 0.0158 0.059 Uiso 1 1 calc R . . H59B H 0.9101 0.2193 0.0658 0.059 Uiso 1 1 calc R . . H59C H 0.9006 0.2467 -0.0041 0.059 Uiso 1 1 calc R . . C61 C 0.5081(4) 0.32226(18) -0.07857(17) 0.0422(9) Uani 1 1 d . . . H61A H 0.4307 0.3194 -0.0615 0.051 Uiso 1 1 calc R . . H61B H 0.5167 0.2837 -0.1048 0.051 Uiso 1 1 calc R . . H61C H 0.5084 0.3623 -0.1038 0.051 Uiso 1 1 calc R . . C62 C 0.7727(4) 0.3561(2) -0.0468(2) 0.0526(11) Uani 1 1 d . . . H62A H 0.7534 0.3993 -0.0659 0.063 Uiso 1 1 calc R . . H62B H 0.7932 0.3253 -0.0785 0.063 Uiso 1 1 calc R . . H62C H 0.8427 0.3602 -0.0134 0.063 Uiso 1 1 calc R . . C71 C 0.5358(4) 0.49198(17) 0.0970(2) 0.0479(10) Uani 1 1 d . . . H71A H 0.5050 0.5098 0.0556 0.057 Uiso 1 1 calc R . . H71B H 0.5634 0.5282 0.1256 0.057 Uiso 1 1 calc R . . H71C H 0.4700 0.4677 0.1130 0.057 Uiso 1 1 calc R . . C72 C 0.7906(4) 0.48218(19) 0.0621(2) 0.0533(11) Uani 1 1 d . . . H72A H 0.8590 0.4524 0.0581 0.064 Uiso 1 1 calc R . . H72B H 0.8190 0.5175 0.0916 0.064 Uiso 1 1 calc R . . H72C H 0.7599 0.5013 0.0212 0.064 Uiso 1 1 calc R . . C81 C 0.8122(3) 0.39955(15) 0.20432(16) 0.0300(7) Uani 1 1 d . . . C82 C 0.9237(3) 0.36444(15) 0.20697(17) 0.0333(8) Uani 1 1 d . . . C83 C 1.0126(3) 0.37047(19) 0.2596(2) 0.0426(9) Uani 1 1 d . . . H83 H 1.0865 0.3460 0.2611 0.051 Uiso 1 1 calc . . . C84 C 0.9980(4) 0.4101(2) 0.3092(2) 0.0477(10) Uani 1 1 d . . . C85 C 0.8906(4) 0.44692(19) 0.30445(19) 0.0463(10) Uani 1 1 d . . . H85 H 0.8798 0.4762 0.3374 0.056 Uiso 1 1 calc . . . C86 C 0.7980(3) 0.44257(17) 0.25318(17) 0.0371(8) Uani 1 1 d . . . C87 C 0.9484(3) 0.32073(17) 0.15409(19) 0.0421(9) Uani 1 1 d . . . H87A H 1.0369 0.3189 0.1529 0.051 Uiso 1 1 calc R . . H87B H 0.9066 0.3385 0.1145 0.051 Uiso 1 1 calc R . . H87C H 0.9178 0.2763 0.1604 0.051 Uiso 1 1 calc R . . C88 C 1.0928(4) 0.4136(3) 0.3675(2) 0.0680(14) Uani 1 1 d . . . H88A H 1.0802 0.3770 0.3953 0.082 Uiso 1 1 calc R . . H88B H 1.0841 0.4554 0.3890 0.082 Uiso 1 1 calc R . . H88C H 1.1752 0.4108 0.3558 0.082 Uiso 1 1 calc R . . C89 C 0.6853(4) 0.4842(2) 0.2517(2) 0.0609(13) Uani 1 1 d . . . H89A H 0.6905 0.5219 0.2240 0.073 Uiso 1 1 calc R . . H89B H 0.6792 0.4999 0.2939 0.073 Uiso 1 1 calc R . . H89C H 0.6127 0.4579 0.2361 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 Th1 0.02167(5) 0.02060(5) 0.02407(6) 0.00149(5) 0.00277(4) -0.00059(5) Si21 0.0202(4) 0.0278(4) 0.0364(5) -0.0003(4) 0.0038(4) -0.0009(4) Si31 0.0225(4) 0.0245(4) 0.0305(5) 0.0058(4) 0.0036(4) 0.0001(3) Si61 0.0390(5) 0.0254(4) 0.0260(5) -0.0002(4) 0.0094(4) 0.0015(4) Si71 0.0445(5) 0.0215(4) 0.0343(6) -0.0009(4) 0.0090(4) -0.0028(4) O11 0.0208(10) 0.0261(10) 0.0306(13) -0.0001(9) 0.0018(9) -0.0008(9) O21 0.0379(12) 0.0241(10) 0.0273(13) 0.0001(9) 0.0089(10) 0.0017(9) N11 0.0233(12) 0.0258(13) 0.0317(16) -0.0004(11) 0.0034(11) 0.0027(10) N41 0.0196(12) 0.0285(13) 0.0318(16) 0.0073(11) 0.0005(11) -0.0010(11) N51 0.0299(14) 0.0231(12) 0.0288(16) 0.0010(11) 0.0038(11) 0.0020(11) N81 0.0335(14) 0.0268(13) 0.0288(16) -0.0017(11) 0.0058(12) -0.0050(12) C11 0.0249(15) 0.0229(14) 0.0306(18) -0.0019(13) 0.0057(13) -0.0003(12) C12 0.0339(17) 0.0298(16) 0.032(2) -0.0007(14) 0.0056(15) 0.0032(14) C13 0.0272(16) 0.0331(17) 0.041(2) 0.0030(15) 0.0044(15) 0.0035(14) C14 0.0334(18) 0.0270(16) 0.048(2) -0.0049(15) 0.0163(16) -0.0004(14) C15 0.045(2) 0.0310(17) 0.039(2) -0.0111(15) 0.0143(17) -0.0030(16) C16 0.0332(17) 0.0311(16) 0.031(2) -0.0041(14) 0.0039(14) -0.0050(14) C17 0.067(3) 0.057(2) 0.030(2) -0.0024(19) 0.0022(19) 0.024(2) C18 0.043(2) 0.0349(19) 0.071(3) -0.0067(19) 0.021(2) 0.0068(17) C19 0.064(3) 0.054(2) 0.036(2) -0.0131(19) -0.009(2) 0.006(2) C21 0.0235(17) 0.041(2) 0.066(3) -0.0105(19) 0.0001(17) 0.0020(16) C22 0.0374(19) 0.047(2) 0.050(3) 0.0069(18) 0.0206(18) 0.0000(17) C31 0.0403(19) 0.0286(16) 0.041(2) 0.0050(15) 0.0075(16) 0.0071(15) C32 0.0352(18) 0.0330(17) 0.038(2) 0.0092(15) 0.0077(15) -0.0030(15) C41 0.0230(15) 0.0382(17) 0.036(2) 0.0218(16) -0.0013(14) -0.0091(14) C42 0.0329(18) 0.051(2) 0.035(2) 0.0158(17) -0.0004(15) -0.0202(17) C43 0.051(3) 0.095(3) 0.036(2) 0.028(2) -0.0108(19) -0.039(3) C44 0.030(2) 0.127(5) 0.058(3) 0.058(3) -0.015(2) -0.027(3) C45 0.0211(18) 0.087(3) 0.080(4) 0.057(3) 0.002(2) -0.001(2) C46 0.0248(17) 0.046(2) 0.064(3) 0.030(2) 0.0034(17) -0.0037(16) C47 0.056(2) 0.046(2) 0.036(2) -0.0022(17) 0.0075(18) -0.0168(19) C48 0.044(3) 0.243(9) 0.072(4) 0.069(5) -0.025(3) -0.029(4) C49 0.030(2) 0.058(3) 0.089(4) 0.015(2) 0.022(2) 0.0106(19) C51 0.0353(17) 0.0239(15) 0.0271(18) -0.0002(13) 0.0048(14) 0.0038(14) C52 0.0399(19) 0.0311(16) 0.0297(19) -0.0035(14) 0.0040(15) -0.0030(15) C53 0.058(2) 0.0318(18) 0.035(2) -0.0055(16) 0.0028(18) -0.0084(18) C54 0.068(3) 0.0290(17) 0.036(2) -0.0050(16) 0.0117(19) 0.0045(18) C55 0.049(2) 0.0340(18) 0.042(2) -0.0052(16) 0.0111(18) 0.0121(17) C56 0.0385(18) 0.0323(17) 0.035(2) -0.0037(15) 0.0063(15) 0.0050(15) C57 0.040(2) 0.047(2) 0.052(3) -0.0100(19) 0.0000(18) -0.0099(18) C58 0.092(4) 0.032(2) 0.064(3) -0.012(2) 0.021(3) 0.002(2) C59 0.0352(19) 0.043(2) 0.071(3) -0.011(2) 0.0073(19) 0.0071(17) C61 0.060(2) 0.042(2) 0.024(2) 0.0002(16) 0.0030(17) 0.0089(18) C62 0.063(3) 0.048(2) 0.053(3) 0.001(2) 0.032(2) -0.003(2) C71 0.069(3) 0.0300(18) 0.044(3) -0.0015(17) 0.005(2) 0.0102(18) C72 0.066(3) 0.038(2) 0.057(3) 0.0043(19) 0.015(2) -0.016(2) C81 0.0330(17) 0.0247(15) 0.033(2) 0.0016(13) 0.0085(14) -0.0071(13) C82 0.0327(17) 0.0274(16) 0.041(2) 0.0082(15) 0.0114(15) -0.0048(14) C83 0.0328(19) 0.045(2) 0.050(3) 0.0152(19) 0.0068(17) 0.0010(16) C84 0.043(2) 0.052(2) 0.045(3) 0.012(2) -0.0044(18) -0.0124(19) C85 0.050(2) 0.043(2) 0.044(3) -0.0093(18) 0.0032(19) -0.0088(19) C86 0.0366(19) 0.0386(18) 0.035(2) -0.0070(16) 0.0025(16) -0.0088(16) C87 0.044(2) 0.0344(18) 0.052(3) 0.0070(17) 0.0186(18) 0.0026(16) C88 0.055(3) 0.090(4) 0.052(3) 0.010(3) -0.013(2) -0.010(3) C89 0.053(3) 0.069(3) 0.058(3) -0.032(2) -0.001(2) 0.015(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; # MOLECULAR GEOMETRY 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 Th1 N41 2.329(2) . ? Th1 N81 2.333(2) . ? Th1 N51 2.336(3) . ? Th1 N11 2.343(2) . ? Th1 O21 2.726(2) . ? Th1 O11 2.741(2) . ? Th1 Si71 3.2785(9) . ? Th1 Si61 3.2949(10) . ? Th1 Si31 3.2949(8) . ? Th1 Si21 3.2968(9) . ? Si21 O11 1.667(2) . ? Si21 N11 1.715(3) . ? Si21 C21 1.857(4) . ? Si21 C22 1.861(4) . ? Si31 O11 1.676(2) . ? Si31 N41 1.720(3) . ? Si31 C31 1.849(3) . ? Si31 C32 1.857(4) . ? Si61 O21 1.672(2) . ? Si61 N51 1.715(3) . ? Si61 C61 1.853(4) . ? Si61 C62 1.854(4) . ? Si71 O21 1.673(2) . ? Si71 N81 1.703(3) . ? Si71 C72 1.851(4) . ? Si71 C71 1.854(4) . ? N11 C11 1.438(4) . ? N41 C41 1.439(4) . ? N51 C51 1.439(4) . ? N81 C81 1.429(4) . ? C11 C16 1.406(5) . ? C11 C12 1.408(5) . ? C12 C13 1.403(4) . ? C12 C17 1.499(5) . ? C13 C14 1.378(5) . ? C13 H13 0.9500 . ? C14 C15 1.382(5) . ? C14 C18 1.506(5) . ? C15 C16 1.396(5) . ? C15 H15 0.9500 . ? C16 C19 1.510(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C41 C42 1.398(6) . ? C41 C46 1.403(5) . ? C42 C43 1.398(5) . ? C42 C47 1.507(6) . ? C43 C44 1.386(8) . ? C43 H43 0.9500 . ? C44 C45 1.361(8) . ? C44 C48 1.527(6) . ? C45 C46 1.402(6) . ? C45 H45 0.9500 . ? C46 C49 1.496(6) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C51 C52 1.409(5) . ? C51 C56 1.412(5) . ? C52 C53 1.401(5) . ? C52 C57 1.506(5) . ? C53 C54 1.375(5) . ? C53 H53 0.9500 . ? C54 C55 1.385(5) . ? C54 C58 1.516(5) . ? C55 C56 1.398(5) . ? C55 H55 0.9500 . ? C56 C59 1.508(5) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C81 C86 1.398(5) . ? C81 C82 1.414(5) . ? C82 C83 1.395(5) . ? C82 C87 1.504(5) . ? C83 C84 1.370(6) . ? C83 H83 0.9500 . ? C84 C85 1.392(6) . ? C84 C88 1.517(6) . ? C85 C86 1.396(5) . ? C85 H85 0.9500 . ? C86 C89 1.498(5) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N41 Th1 N81 118.42(9) . . ? N41 Th1 N51 104.52(9) . . ? N81 Th1 N51 108.47(9) . . ? N41 Th1 N11 108.73(9) . . ? N81 Th1 N11 102.62(9) . . ? N51 Th1 N11 114.50(9) . . ? N41 Th1 O21 158.60(8) . . ? N81 Th1 O21 59.91(8) . . ? N51 Th1 O21 60.07(7) . . ? N11 Th1 O21 91.89(8) . . ? N41 Th1 O11 60.06(7) . . ? N81 Th1 O11 156.34(8) . . ? N51 Th1 O11 94.06(8) . . ? N11 Th1 O11 59.99(7) . . ? O21 Th1 O11 131.10(6) . . ? N41 Th1 Si71 146.04(6) . . ? N81 Th1 Si71 29.67(7) . . ? N51 Th1 Si71 86.43(6) . . ? N11 Th1 Si71 94.89(6) . . ? O21 Th1 Si71 30.64(5) . . ? O11 Th1 Si71 152.57(4) . . ? N41 Th1 Si61 132.34(7) . . ? N81 Th1 Si61 83.63(7) . . ? N51 Th1 Si61 29.68(6) . . ? N11 Th1 Si61 106.03(7) . . ? O21 Th1 Si61 30.41(5) . . ? O11 Th1 Si61 115.38(5) . . ? Si71 Th1 Si61 57.82(2) . . ? N41 Th1 Si31 29.76(6) . . ? N81 Th1 Si31 144.92(7) . . ? N51 Th1 Si31 98.20(6) . . ? N11 Th1 Si31 85.86(6) . . ? O21 Th1 Si31 154.83(5) . . ? O11 Th1 Si31 30.51(4) . . ? Si71 Th1 Si31 174.53(2) . . ? Si61 Th1 Si31 127.17(2) . . ? N41 Th1 Si21 83.66(6) . . ? N81 Th1 Si21 130.17(7) . . ? N51 Th1 Si21 107.52(6) . . ? N11 Th1 Si21 29.72(6) . . ? O21 Th1 Si21 114.18(5) . . ? O11 Th1 Si21 30.31(4) . . ? Si71 Th1 Si21 124.17(2) . . ? Si61 Th1 Si21 115.16(2) . . ? Si31 Th1 Si21 57.24(2) . . ? O11 Si21 N11 98.63(11) . . ? O11 Si21 C21 109.37(14) . . ? N11 Si21 C21 116.52(16) . . ? O11 Si21 C22 110.97(15) . . ? N11 Si21 C22 115.24(16) . . ? C21 Si21 C22 105.95(19) . . ? O11 Si21 Th1 56.08(7) . . ? C21 Si21 Th1 129.38(14) . . ? C22 Si21 Th1 124.66(13) . . ? O11 Si31 N41 97.99(11) . . ? O11 Si31 C31 104.98(14) . . ? N41 Si31 C31 118.18(15) . . ? O11 Si31 C32 113.20(14) . . ? N41 Si31 C32 112.76(15) . . ? C31 Si31 C32 109.09(16) . . ? O11 Si31 Th1 56.15(7) . . ? C31 Si31 Th1 119.70(12) . . ? C32 Si31 Th1 131.20(12) . . ? O21 Si61 N51 98.00(13) . . ? O21 Si61 C61 110.43(15) . . ? N51 Si61 C61 114.21(15) . . ? O21 Si61 C62 109.16(16) . . ? N51 Si61 C62 117.85(17) . . ? C61 Si61 C62 106.8(2) . . ? O21 Si61 Th1 55.63(8) . . ? C61 Si61 Th1 127.30(13) . . ? C62 Si61 Th1 125.89(15) . . ? O21 Si71 N81 98.03(12) . . ? O21 Si71 C72 113.13(17) . . ? N81 Si71 C72 113.54(18) . . ? O21 Si71 C71 104.55(15) . . ? N81 Si71 C71 117.61(17) . . ? C72 Si71 C71 109.21(19) . . ? O21 Si71 Th1 56.12(8) . . ? C72 Si71 Th1 133.91(14) . . ? C71 Si71 Th1 116.88(14) . . ? Si21 O11 Si31 141.64(15) . . ? Si21 O11 Th1 93.61(9) . . ? Si31 O11 Th1 93.34(8) . . ? Si61 O21 Si71 143.59(15) . . ? Si61 O21 Th1 93.95(9) . . ? Si71 O21 Th1 93.25(10) . . ? C11 N11 Si21 118.7(2) . . ? C11 N11 Th1 133.60(19) . . ? Si21 N11 Th1 107.64(12) . . ? C41 N41 Si31 121.0(2) . . ? C41 N41 Th1 129.04(19) . . ? Si31 N41 Th1 108.01(12) . . ? C51 N51 Si61 123.6(2) . . ? C51 N51 Th1 128.4(2) . . ? Si61 N51 Th1 107.89(12) . . ? C81 N81 Si71 128.5(2) . . ? C81 N81 Th1 122.14(19) . . ? Si71 N81 Th1 107.65(13) . . ? C16 C11 C12 118.8(3) . . ? C16 C11 N11 121.3(3) . . ? C12 C11 N11 119.9(3) . . ? C13 C12 C11 119.2(3) . . ? C13 C12 C17 118.8(3) . . ? C11 C12 C17 122.0(3) . . ? C14 C13 C12 123.0(3) . . ? C14 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? C13 C14 C15 116.5(3) . . ? C13 C14 C18 122.1(4) . . ? C15 C14 C18 121.4(3) . . ? C14 C15 C16 123.5(3) . . ? C14 C15 H15 118.2 . . ? C16 C15 H15 118.2 . . ? C15 C16 C11 118.9(3) . . ? C15 C16 C19 119.0(3) . . ? C11 C16 C19 122.1(3) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si21 C21 H21A 109.5 . . ? Si21 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si21 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si21 C22 H22A 109.5 . . ? Si21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si31 C31 H31A 109.5 . . ? Si31 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si31 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si31 C32 H32A 109.5 . . ? Si31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C42 C41 C46 119.8(3) . . ? C42 C41 N41 119.3(3) . . ? C46 C41 N41 120.9(4) . . ? C43 C42 C41 119.4(4) . . ? C43 C42 C47 119.0(4) . . ? C41 C42 C47 121.6(3) . . ? C44 C43 C42 121.3(5) . . ? C44 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? C45 C44 C43 118.4(4) . . ? C45 C44 C48 121.5(6) . . ? C43 C44 C48 120.1(6) . . ? C44 C45 C46 122.8(4) . . ? C44 C45 H45 118.6 . . ? C46 C45 H45 118.6 . . ? C45 C46 C41 118.2(4) . . ? C45 C46 C49 119.5(4) . . ? C41 C46 C49 122.2(3) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C52 C51 C56 118.5(3) . . ? C52 C51 N51 121.0(3) . . ? C56 C51 N51 120.5(3) . . ? C53 C52 C51 119.7(3) . . ? C53 C52 C57 118.4(3) . . ? C51 C52 C57 121.9(3) . . ? C54 C53 C52 122.2(3) . . ? C54 C53 H53 118.9 . . ? C52 C53 H53 118.9 . . ? C53 C54 C55 117.9(3) . . ? C53 C54 C58 121.5(4) . . ? C55 C54 C58 120.6(4) . . ? C54 C55 C56 122.3(3) . . ? C54 C55 H55 118.8 . . ? C56 C55 H55 118.8 . . ? C55 C56 C51 119.4(3) . . ? C55 C56 C59 118.6(3) . . ? C51 C56 C59 122.0(3) . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C54 C58 H58A 109.5 . . ? C54 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C54 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C56 C59 H59A 109.5 . . ? C56 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C56 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? Si61 C61 H61A 109.5 . . ? Si61 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? Si61 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? Si61 C62 H62A 109.5 . . ? Si61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? Si61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? Si71 C71 H71A 109.5 . . ? Si71 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? Si71 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? Si71 C72 H72A 109.5 . . ? Si71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? Si71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C86 C81 C82 118.5(3) . . ? C86 C81 N81 122.2(3) . . ? C82 C81 N81 119.2(3) . . ? C83 C82 C81 119.4(3) . . ? C83 C82 C87 119.3(3) . . ? C81 C82 C87 121.3(3) . . ? C84 C83 C82 122.9(3) . . ? C84 C83 H83 118.6 . . ? C82 C83 H83 118.6 . . ? C83 C84 C85 117.0(4) . . ? C83 C84 C88 122.3(4) . . ? C85 C84 C88 120.7(4) . . ? C84 C85 C86 122.6(4) . . ? C84 C85 H85 118.7 . . ? C86 C85 H85 118.7 . . ? C85 C86 C81 119.4(3) . . ? C85 C86 C89 119.2(3) . . ? C81 C86 C89 121.4(3) . . ? C82 C87 H87A 109.5 . . ? C82 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C82 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C84 C88 H88A 109.5 . . ? C84 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C84 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C86 C89 H89A 109.5 . . ? C86 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C86 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 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 N41 Th1 Si21 O11 -36.41(12) . . . . ? N81 Th1 Si21 O11 -158.61(13) . . . . ? N51 Th1 Si21 O11 66.86(11) . . . . ? N11 Th1 Si21 O11 175.78(17) . . . . ? O21 Th1 Si21 O11 131.28(11) . . . . ? Si71 Th1 Si21 O11 164.65(9) . . . . ? Si61 Th1 Si21 O11 97.74(10) . . . . ? Si31 Th1 Si21 O11 -21.69(9) . . . . ? N41 Th1 Si21 N11 147.82(16) . . . . ? N81 Th1 Si21 N11 25.62(17) . . . . ? N51 Th1 Si21 N11 -108.91(15) . . . . ? O21 Th1 Si21 N11 -44.50(15) . . . . ? O11 Th1 Si21 N11 -175.78(17) . . . . ? Si71 Th1 Si21 N11 -11.13(14) . . . . ? Si61 Th1 Si21 N11 -78.03(14) . . . . ? Si31 Th1 Si21 N11 162.53(14) . . . . ? N41 Th1 Si21 C21 -124.40(17) . . . . ? N81 Th1 Si21 C21 113.40(18) . . . . ? N51 Th1 Si21 C21 -21.13(17) . . . . ? N11 Th1 Si21 C21 87.8(2) . . . . ? O21 Th1 Si21 C21 43.29(16) . . . . ? O11 Th1 Si21 C21 -88.00(18) . . . . ? Si71 Th1 Si21 C21 76.65(16) . . . . ? Si61 Th1 Si21 C21 9.75(16) . . . . ? Si31 Th1 Si21 C21 -109.69(16) . . . . ? N41 Th1 Si21 C22 56.99(17) . . . . ? N81 Th1 Si21 C22 -65.21(18) . . . . ? N51 Th1 Si21 C22 160.26(16) . . . . ? N11 Th1 Si21 C22 -90.8(2) . . . . ? O21 Th1 Si21 C22 -135.32(16) . . . . ? O11 Th1 Si21 C22 93.40(18) . . . . ? Si71 Th1 Si21 C22 -101.95(15) . . . . ? Si61 Th1 Si21 C22 -168.86(15) . . . . ? Si31 Th1 Si21 C22 71.71(15) . . . . ? N41 Th1 Si31 O11 170.98(18) . . . . ? N81 Th1 Si31 O11 136.28(15) . . . . ? N51 Th1 Si31 O11 -84.05(11) . . . . ? N11 Th1 Si31 O11 30.14(11) . . . . ? O21 Th1 Si31 O11 -55.49(15) . . . . ? Si61 Th1 Si31 O11 -76.87(10) . . . . ? Si21 Th1 Si31 O11 21.56(9) . . . . ? N81 Th1 Si31 N41 -34.70(19) . . . . ? N51 Th1 Si31 N41 104.97(16) . . . . ? N11 Th1 Si31 N41 -140.85(16) . . . . ? O21 Th1 Si31 N41 133.53(18) . . . . ? O11 Th1 Si31 N41 -170.98(18) . . . . ? Si61 Th1 Si31 N41 112.15(14) . . . . ? Si21 Th1 Si31 N41 -149.43(15) . . . . ? N41 Th1 Si31 C31 -100.4(2) . . . . ? N81 Th1 Si31 C31 -135.10(17) . . . . ? N51 Th1 Si31 C31 4.57(15) . . . . ? N11 Th1 Si31 C31 118.75(15) . . . . ? O21 Th1 Si31 C31 33.12(18) . . . . ? O11 Th1 Si31 C31 88.61(16) . . . . ? Si61 Th1 Si31 C31 11.75(14) . . . . ? Si21 Th1 Si31 C31 110.17(14) . . . . ? N41 Th1 Si31 C32 78.5(2) . . . . ? N81 Th1 Si31 C32 43.8(2) . . . . ? N51 Th1 Si31 C32 -176.53(16) . . . . ? N11 Th1 Si31 C32 -62.34(16) . . . . ? O21 Th1 Si31 C32 -147.97(18) . . . . ? O11 Th1 Si31 C32 -92.48(18) . . . . ? Si61 Th1 Si31 C32 -169.35(15) . . . . ? Si21 Th1 Si31 C32 -70.93(15) . . . . ? N41 Th1 Si61 O21 -159.37(12) . . . . ? N81 Th1 Si61 O21 -36.27(12) . . . . ? N51 Th1 Si61 O21 176.63(17) . . . . ? N11 Th1 Si61 O21 65.07(12) . . . . ? O11 Th1 Si61 O21 128.99(11) . . . . ? Si71 Th1 Si61 O21 -20.57(10) . . . . ? Si31 Th1 Si61 O21 162.16(10) . . . . ? Si21 Th1 Si61 O21 95.38(10) . . . . ? N41 Th1 Si61 N51 24.00(15) . . . . ? N81 Th1 Si61 N51 147.10(15) . . . . ? N11 Th1 Si61 N51 -111.55(14) . . . . ? O21 Th1 Si61 N51 -176.63(17) . . . . ? O11 Th1 Si61 N51 -47.64(14) . . . . ? Si71 Th1 Si61 N51 162.80(13) . . . . ? Si31 Th1 Si61 N51 -14.46(13) . . . . ? Si21 Th1 Si61 N51 -81.24(13) . . . . ? N41 Th1 Si61 C61 110.01(17) . . . . ? N81 Th1 Si61 C61 -126.88(16) . . . . ? N51 Th1 Si61 C61 86.0(2) . . . . ? N11 Th1 Si61 C61 -25.54(16) . . . . ? O21 Th1 Si61 C61 -90.61(18) . . . . ? O11 Th1 Si61 C61 38.38(16) . . . . ? Si71 Th1 Si61 C61 -111.19(15) . . . . ? Si31 Th1 Si61 C61 71.55(15) . . . . ? Si21 Th1 Si61 C61 4.77(15) . . . . ? N41 Th1 Si61 C62 -69.61(18) . . . . ? N81 Th1 Si61 C62 53.49(18) . . . . ? N51 Th1 Si61 C62 -93.6(2) . . . . ? N11 Th1 Si61 C62 154.83(17) . . . . ? O21 Th1 Si61 C62 89.76(19) . . . . ? O11 Th1 Si61 C62 -141.25(17) . . . . ? Si71 Th1 Si61 C62 69.19(16) . . . . ? Si31 Th1 Si61 C62 -108.07(16) . . . . ? Si21 Th1 Si61 C62 -174.86(16) . . . . ? N41 Th1 Si71 O21 139.80(15) . . . . ? N81 Th1 Si71 O21 167.53(17) . . . . ? N51 Th1 Si71 O21 28.87(11) . . . . ? N11 Th1 Si71 O21 -85.44(12) . . . . ? O11 Th1 Si71 O21 -63.07(14) . . . . ? Si61 Th1 Si71 O21 20.43(9) . . . . ? Si21 Th1 Si71 O21 -79.93(10) . . . . ? N41 Th1 Si71 N81 -27.73(19) . . . . ? N51 Th1 Si71 N81 -138.66(15) . . . . ? N11 Th1 Si71 N81 107.02(15) . . . . ? O21 Th1 Si71 N81 -167.53(17) . . . . ? O11 Th1 Si71 N81 129.40(17) . . . . ? Si61 Th1 Si71 N81 -147.10(14) . . . . ? Si21 Th1 Si71 N81 112.54(14) . . . . ? N41 Th1 Si71 C72 49.2(2) . . . . ? N81 Th1 Si71 C72 76.9(2) . . . . ? N51 Th1 Si71 C72 -61.7(2) . . . . ? N11 Th1 Si71 C72 -176.0(2) . . . . ? O21 Th1 Si71 C72 -90.6(2) . . . . ? O11 Th1 Si71 C72 -153.7(2) . . . . ? Si61 Th1 Si71 C72 -70.2(2) . . . . ? Si21 Th1 Si71 C72 -170.5(2) . . . . ? N41 Th1 Si71 C71 -130.26(19) . . . . ? N81 Th1 Si71 C71 -102.5(2) . . . . ? N51 Th1 Si71 C71 118.82(16) . . . . ? N11 Th1 Si71 C71 4.50(16) . . . . ? O21 Th1 Si71 C71 89.94(18) . . . . ? O11 Th1 Si71 C71 26.87(19) . . . . ? Si61 Th1 Si71 C71 110.38(15) . . . . ? Si21 Th1 Si71 C71 10.01(16) . . . . ? N11 Si21 O11 Si31 102.9(2) . . . . ? C21 Si21 O11 Si31 -135.0(2) . . . . ? C22 Si21 O11 Si31 -18.4(3) . . . . ? Th1 Si21 O11 Si31 100.0(2) . . . . ? N11 Si21 O11 Th1 2.89(12) . . . . ? C21 Si21 O11 Th1 125.03(15) . . . . ? C22 Si21 O11 Th1 -118.44(14) . . . . ? N41 Si31 O11 Si21 -94.0(2) . . . . ? C31 Si31 O11 Si21 143.9(2) . . . . ? C32 Si31 O11 Si21 25.0(3) . . . . ? Th1 Si31 O11 Si21 -100.1(2) . . . . ? N41 Si31 O11 Th1 6.11(12) . . . . ? C31 Si31 O11 Th1 -115.98(13) . . . . ? C32 Si31 O11 Th1 125.13(13) . . . . ? N41 Th1 O11 Si21 137.10(13) . . . . ? N81 Th1 O11 Si21 44.0(2) . . . . ? N51 Th1 O11 Si21 -118.47(10) . . . . ? N11 Th1 O11 Si21 -2.42(10) . . . . ? O21 Th1 O11 Si21 -65.47(12) . . . . ? Si71 Th1 O11 Si21 -28.39(17) . . . . ? Si61 Th1 O11 Si21 -96.95(9) . . . . ? Si31 Th1 O11 Si21 142.25(16) . . . . ? N41 Th1 O11 Si31 -5.15(10) . . . . ? N81 Th1 O11 Si31 -98.3(2) . . . . ? N51 Th1 O11 Si31 99.28(10) . . . . ? N11 Th1 O11 Si31 -144.67(13) . . . . ? O21 Th1 O11 Si31 152.28(8) . . . . ? Si71 Th1 O11 Si31 -170.64(5) . . . . ? Si61 Th1 O11 Si31 120.80(8) . . . . ? Si21 Th1 O11 Si31 -142.25(16) . . . . ? N51 Si61 O21 Si71 103.2(2) . . . . ? C61 Si61 O21 Si71 -137.2(2) . . . . ? C62 Si61 O21 Si71 -20.0(3) . . . . ? Th1 Si61 O21 Si71 100.9(2) . . . . ? N51 Si61 O21 Th1 2.30(11) . . . . ? C61 Si61 O21 Th1 121.91(14) . . . . ? C62 Si61 O21 Th1 -120.95(16) . . . . ? N81 Si71 O21 Si61 -92.6(3) . . . . ? C72 Si71 O21 Si61 27.3(3) . . . . ? C71 Si71 O21 Si61 146.0(3) . . . . ? Th1 Si71 O21 Si61 -101.1(2) . . . . ? N81 Si71 O21 Th1 8.50(12) . . . . ? C72 Si71 O21 Th1 128.43(16) . . . . ? C71 Si71 O21 Th1 -112.85(15) . . . . ? N41 Th1 O21 Si61 45.5(3) . . . . ? N81 Th1 O21 Si61 137.20(13) . . . . ? N51 Th1 O21 Si61 -1.93(9) . . . . ? N11 Th1 O21 Si61 -119.30(11) . . . . ? O11 Th1 O21 Si61 -68.74(12) . . . . ? Si71 Th1 O21 Si61 144.29(16) . . . . ? Si31 Th1 O21 Si61 -35.02(18) . . . . ? Si21 Th1 O21 Si61 -98.95(9) . . . . ? N41 Th1 O21 Si71 -98.8(2) . . . . ? N81 Th1 O21 Si71 -7.09(10) . . . . ? N51 Th1 O21 Si71 -146.22(13) . . . . ? N11 Th1 O21 Si71 96.41(11) . . . . ? O11 Th1 O21 Si71 146.97(8) . . . . ? Si61 Th1 O21 Si71 -144.29(16) . . . . ? Si31 Th1 O21 Si71 -179.31(5) . . . . ? Si21 Th1 O21 Si71 116.76(8) . . . . ? O11 Si21 N11 C11 177.8(2) . . . . ? C21 Si21 N11 C11 61.0(3) . . . . ? C22 Si21 N11 C11 -64.0(3) . . . . ? Th1 Si21 N11 C11 -178.6(3) . . . . ? O11 Si21 N11 Th1 -3.54(15) . . . . ? C21 Si21 N11 Th1 -120.32(17) . . . . ? C22 Si21 N11 Th1 114.60(16) . . . . ? N41 Th1 N11 C11 144.4(3) . . . . ? N81 Th1 N11 C11 18.1(3) . . . . ? N51 Th1 N11 C11 -99.2(3) . . . . ? O21 Th1 N11 C11 -41.4(3) . . . . ? O11 Th1 N11 C11 -179.2(3) . . . . ? Si71 Th1 N11 C11 -10.9(3) . . . . ? Si61 Th1 N11 C11 -68.8(3) . . . . ? Si31 Th1 N11 C11 163.7(3) . . . . ? Si21 Th1 N11 C11 178.3(4) . . . . ? N41 Th1 N11 Si21 -33.99(16) . . . . ? N81 Th1 N11 Si21 -160.21(13) . . . . ? N51 Th1 N11 Si21 82.48(15) . . . . ? O21 Th1 N11 Si21 140.23(13) . . . . ? O11 Th1 N11 Si21 2.46(10) . . . . ? Si71 Th1 N11 Si21 170.78(12) . . . . ? Si61 Th1 N11 Si21 112.89(12) . . . . ? Si31 Th1 N11 Si21 -14.66(12) . . . . ? O11 Si31 N41 C41 157.9(3) . . . . ? C31 Si31 N41 C41 -90.3(3) . . . . ? C32 Si31 N41 C41 38.5(3) . . . . ? Th1 Si31 N41 C41 165.4(3) . . . . ? O11 Si31 N41 Th1 -7.55(15) . . . . ? C31 Si31 N41 Th1 104.24(16) . . . . ? C32 Si31 N41 Th1 -126.91(15) . . . . ? N81 Th1 N41 C41 -5.7(3) . . . . ? N51 Th1 N41 C41 115.1(3) . . . . ? N11 Th1 N41 C41 -122.2(3) . . . . ? O21 Th1 N41 C41 73.8(4) . . . . ? O11 Th1 N41 C41 -158.6(3) . . . . ? Si71 Th1 N41 C41 9.5(4) . . . . ? Si61 Th1 N41 C41 103.1(3) . . . . ? Si31 Th1 N41 C41 -163.9(4) . . . . ? Si21 Th1 N41 C41 -138.4(3) . . . . ? N81 Th1 N41 Si31 158.16(12) . . . . ? N51 Th1 N41 Si31 -81.02(14) . . . . ? N11 Th1 N41 Si31 41.68(16) . . . . ? O21 Th1 N41 Si31 -122.29(18) . . . . ? O11 Th1 N41 Si31 5.27(10) . . . . ? Si71 Th1 N41 Si31 173.34(5) . . . . ? Si61 Th1 N41 Si31 -93.03(13) . . . . ? Si21 Th1 N41 Si31 25.49(12) . . . . ? O21 Si61 N51 C51 173.6(2) . . . . ? C61 Si61 N51 C51 56.9(3) . . . . ? C62 Si61 N51 C51 -69.7(3) . . . . ? Th1 Si61 N51 C51 176.4(3) . . . . ? O21 Si61 N51 Th1 -2.81(14) . . . . ? C61 Si61 N51 Th1 -119.54(16) . . . . ? C62 Si61 N51 Th1 113.87(18) . . . . ? N41 Th1 N51 C51 21.9(3) . . . . ? N81 Th1 N51 C51 149.1(2) . . . . ? N11 Th1 N51 C51 -97.0(3) . . . . ? O21 Th1 N51 C51 -174.2(3) . . . . ? O11 Th1 N51 C51 -38.2(2) . . . . ? Si71 Th1 N51 C51 169.3(2) . . . . ? Si61 Th1 N51 C51 -176.2(3) . . . . ? Si31 Th1 N51 C51 -7.8(3) . . . . ? Si21 Th1 N51 C51 -65.9(2) . . . . ? N41 Th1 N51 Si61 -161.91(12) . . . . ? N81 Th1 N51 Si61 -34.69(15) . . . . ? N11 Th1 N51 Si61 79.23(14) . . . . ? O21 Th1 N51 Si61 1.97(10) . . . . ? O11 Th1 N51 Si61 137.99(12) . . . . ? Si71 Th1 N51 Si61 -14.53(11) . . . . ? Si31 Th1 N51 Si61 168.40(11) . . . . ? Si21 Th1 N51 Si61 110.26(11) . . . . ? O21 Si71 N81 C81 154.9(3) . . . . ? C72 Si71 N81 C81 35.2(3) . . . . ? C71 Si71 N81 C81 -94.0(3) . . . . ? Th1 Si71 N81 C81 165.3(4) . . . . ? O21 Si71 N81 Th1 -10.43(14) . . . . ? C72 Si71 N81 Th1 -130.05(17) . . . . ? C71 Si71 N81 Th1 100.69(18) . . . . ? N41 Th1 N81 C81 -3.6(3) . . . . ? N51 Th1 N81 C81 -122.4(2) . . . . ? N11 Th1 N81 C81 116.1(2) . . . . ? O21 Th1 N81 C81 -159.1(3) . . . . ? O11 Th1 N81 C81 76.1(3) . . . . ? Si71 Th1 N81 C81 -166.4(3) . . . . ? Si61 Th1 N81 C81 -138.9(2) . . . . ? Si31 Th1 N81 C81 15.1(3) . . . . ? Si21 Th1 N81 C81 103.4(2) . . . . ? N41 Th1 N81 Si71 162.81(12) . . . . ? N51 Th1 N81 Si71 44.03(15) . . . . ? N11 Th1 N81 Si71 -77.50(14) . . . . ? O21 Th1 N81 Si71 7.30(10) . . . . ? O11 Th1 N81 Si71 -117.49(18) . . . . ? Si61 Th1 N81 Si71 27.56(12) . . . . ? Si31 Th1 N81 Si71 -178.45(5) . . . . ? Si21 Th1 N81 Si71 -90.19(14) . . . . ? Si21 N11 C11 C16 89.6(3) . . . . ? Th1 N11 C11 C16 -88.6(4) . . . . ? Si21 N11 C11 C12 -90.1(3) . . . . ? Th1 N11 C11 C12 91.7(3) . . . . ? C16 C11 C12 C13 -2.3(5) . . . . ? N11 C11 C12 C13 177.4(3) . . . . ? C16 C11 C12 C17 175.7(3) . . . . ? N11 C11 C12 C17 -4.6(5) . . . . ? C11 C12 C13 C14 0.4(5) . . . . ? C17 C12 C13 C14 -177.7(4) . . . . ? C12 C13 C14 C15 1.5(5) . . . . ? C12 C13 C14 C18 -177.3(3) . . . . ? C13 C14 C15 C16 -1.5(5) . . . . ? C18 C14 C15 C16 177.3(3) . . . . ? C14 C15 C16 C11 -0.3(5) . . . . ? C14 C15 C16 C19 179.7(4) . . . . ? C12 C11 C16 C15 2.2(5) . . . . ? N11 C11 C16 C15 -177.5(3) . . . . ? C12 C11 C16 C19 -177.8(3) . . . . ? N11 C11 C16 C19 2.6(5) . . . . ? Si31 N41 C41 C42 -100.1(3) . . . . ? Th1 N41 C41 C42 61.9(4) . . . . ? Si31 N41 C41 C46 81.4(4) . . . . ? Th1 N41 C41 C46 -116.5(3) . . . . ? C46 C41 C42 C43 0.4(5) . . . . ? N41 C41 C42 C43 -178.0(3) . . . . ? C46 C41 C42 C47 179.1(3) . . . . ? N41 C41 C42 C47 0.6(5) . . . . ? C41 C42 C43 C44 -1.1(6) . . . . ? C47 C42 C43 C44 -179.8(4) . . . . ? C42 C43 C44 C45 0.6(6) . . . . ? C42 C43 C44 C48 179.9(4) . . . . ? C43 C44 C45 C46 0.7(7) . . . . ? C48 C44 C45 C46 -178.6(4) . . . . ? C44 C45 C46 C41 -1.3(6) . . . . ? C44 C45 C46 C49 179.7(4) . . . . ? C42 C41 C46 C45 0.8(5) . . . . ? N41 C41 C46 C45 179.2(3) . . . . ? C42 C41 C46 C49 179.7(3) . . . . ? N41 C41 C46 C49 -1.9(5) . . . . ? Si61 N51 C51 C52 -91.1(4) . . . . ? Th1 N51 C51 C52 84.6(4) . . . . ? Si61 N51 C51 C56 92.5(3) . . . . ? Th1 N51 C51 C56 -91.9(3) . . . . ? C56 C51 C52 C53 2.0(5) . . . . ? N51 C51 C52 C53 -174.5(3) . . . . ? C56 C51 C52 C57 -179.4(3) . . . . ? N51 C51 C52 C57 4.1(5) . . . . ? C51 C52 C53 C54 0.6(6) . . . . ? C57 C52 C53 C54 -178.1(4) . . . . ? C52 C53 C54 C55 -2.7(6) . . . . ? C52 C53 C54 C58 175.5(4) . . . . ? C53 C54 C55 C56 2.2(6) . . . . ? C58 C54 C55 C56 -176.0(4) . . . . ? C54 C55 C56 C51 0.3(6) . . . . ? C54 C55 C56 C59 -179.9(4) . . . . ? C52 C51 C56 C55 -2.4(5) . . . . ? N51 C51 C56 C55 174.1(3) . . . . ? C52 C51 C56 C59 177.8(4) . . . . ? N51 C51 C56 C59 -5.7(5) . . . . ? Si71 N81 C81 C86 77.1(4) . . . . ? Th1 N81 C81 C86 -119.5(3) . . . . ? Si71 N81 C81 C82 -106.6(3) . . . . ? Th1 N81 C81 C82 56.8(4) . . . . ? C86 C81 C82 C83 4.0(5) . . . . ? N81 C81 C82 C83 -172.5(3) . . . . ? C86 C81 C82 C87 -176.0(3) . . . . ? N81 C81 C82 C87 7.6(5) . . . . ? C81 C82 C83 C84 -1.1(5) . . . . ? C87 C82 C83 C84 178.9(3) . . . . ? C82 C83 C84 C85 -2.2(6) . . . . ? C82 C83 C84 C88 177.0(4) . . . . ? C83 C84 C85 C86 2.7(6) . . . . ? C88 C84 C85 C86 -176.5(4) . . . . ? C84 C85 C86 C81 0.2(6) . . . . ? C84 C85 C86 C89 -179.8(4) . . . . ? C82 C81 C86 C85 -3.5(5) . . . . ? N81 C81 C86 C85 172.8(3) . . . . ? C82 C81 C86 C89 176.5(4) . . . . ? N81 C81 C86 C89 -7.2(5) . . . . ?