# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address 'David Emslie' ;Department of Chemistry and Chemical Biology McMaster University 1280 Main Street West Hamilton, ON, L8S 4M1 Canada ; 'James F Britten' ;Department of Chemistry and Chemical Biology McMaster University 1280 Main Street West Hamilton, ON, L8S 4M1 Canada ; 'Carlos A. Cruz' ;Department of Chemistry and Chemical Biology McMaster University 1280 Main Street West Hamilton, ON, L8S 4M1 Canada ; 'Hilary A. Jenkins' ;Department of Chemistry and Chemical Biology McMaster University 1280 Main Street West Hamilton, ON, L8S 4M1 Canada ; _publ_contact_author_name 'David Emslie' _publ_contact_author_email EMSLIED@MCMASTER.CA _publ_section_title ; A Thermally Robust Di-n-Butyl Thorium Complex with an Unstable Dimethyl Analogue ; _publ_contact_author_address ;Department of Chemistry and Chemical Biology McMaster University 1280 Main Street West Hamilton, ON, L8S 4M1 Canada ; _publ_contact_author_fax 905-522-2509 _publ_contact_author_phone '905-525-9140 x 23307' # Attachment 'Th_complex_3.cif' data_cruz50 _database_code_depnum_ccdc_archive 'CCDC 756442' _publ_section_abstract ; Methyl and n-butyl thorium complexes of a rigid 2,6-bis(anilidomethyl)pyridine ligand have been prepared; the n butyl complex is thermally stable, even at 80 oC, while the methyl complexes exhibit a high tendency to eliminate methane via sigma-bond metathesis. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C37 H56 Li N3 O2 Th, C6 H14' _chemical_formula_sum 'C43 H70 Li N3 O2 Th' _exptl_crystal_recrystallization_method 'toluene/hexane, -30 oC' _chemical_melting_point ? _exptl_crystal_description rod _exptl_crystal_colour orange _diffrn_ambient_temperature 173(2) _chemical_formula_weight 900.02 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_int_tables_number 15 _chemical_absolute_configuration ? _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.258(7) _cell_length_b 14.286(3) _cell_length_c 17.419(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.922(4) _cell_angle_gamma 90.00 _cell_volume 8309(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1355 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 14.09 _exptl_crystal_size_max 0.126 _exptl_crystal_size_mid 0.097 _exptl_crystal_size_min 0.031 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 3.622 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6561 _exptl_absorpt_correction_T_max 0.9402 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41676 _diffrn_reflns_av_R_equivalents 0.1567 _diffrn_reflns_av_sigmaI/netI 0.1348 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7306 _reflns_number_gt 4040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7306 _refine_ls_number_parameters 386 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1322 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.1447 _refine_ls_wR_factor_gt 0.1268 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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 0.149064(13) 0.36398(3) 0.17279(2) 0.04312(16) Uani 1 1 d . . . N1 N 0.1679(3) 0.2356(6) 0.2525(5) 0.045(2) Uani 1 1 d . A . N2 N 0.2155(3) 0.3782(6) 0.2809(5) 0.042(2) Uani 1 1 d . A . N3 N 0.1838(3) 0.5059(6) 0.1758(5) 0.044(2) Uani 1 1 d . A . C1 C 0.1488(4) 0.1555(7) 0.2102(7) 0.055(3) Uani 1 1 d . A . C2 C 0.1471(3) 0.1553(7) 0.1257(7) 0.043(3) Uani 1 1 d . . . C3 C 0.1244(4) 0.0828(8) 0.0808(7) 0.055(3) Uani 1 1 d . A . H3A H 0.1220 0.0817 0.0254 0.065 Uiso 1 1 calc R . . C4 C 0.1057(4) 0.0135(8) 0.1156(8) 0.058(3) Uani 1 1 d . . . H4A H 0.0909 -0.0341 0.0837 0.069 Uiso 1 1 calc R A . C5 C 0.1085(4) 0.0130(8) 0.1954(8) 0.059(3) Uani 1 1 d . A . H5A H 0.0970 -0.0372 0.2186 0.071 Uiso 1 1 calc R . . C6 C 0.1279(4) 0.0858(8) 0.2432(7) 0.049(3) Uani 1 1 d . . . C7 C 0.1687(4) 0.2305(8) 0.0904(6) 0.051(3) Uani 1 1 d . A . C8 C 0.1592(5) 0.2234(9) -0.0006(7) 0.090(5) Uani 1 1 d . . . H8A H 0.1703 0.1649 -0.0162 0.135 Uiso 1 1 calc R A . H8B H 0.1713 0.2766 -0.0223 0.135 Uiso 1 1 calc R . . H8C H 0.1301 0.2241 -0.0210 0.135 Uiso 1 1 calc R . . C9 C 0.2137(4) 0.2293(8) 0.1192(8) 0.072(4) Uani 1 1 d . . . H9A H 0.2250 0.1799 0.0919 0.108 Uiso 1 1 calc R A . H9B H 0.2205 0.2173 0.1761 0.108 Uiso 1 1 calc R . . H9C H 0.2246 0.2900 0.1085 0.108 Uiso 1 1 calc R . . C10 C 0.1263(4) 0.0920(8) 0.3305(7) 0.059(3) Uani 1 1 d . A . H10A H 0.1365 0.1552 0.3500 0.071 Uiso 1 1 calc R . . C11 C 0.1549(5) 0.0183(9) 0.3778(8) 0.094(5) Uani 1 1 d . . . H11A H 0.1540 0.0224 0.4336 0.141 Uiso 1 1 calc R A . H11B H 0.1822 0.0302 0.3720 0.141 Uiso 1 1 calc R . . H11C H 0.1465 -0.0444 0.3579 0.141 Uiso 1 1 calc R . . C12 C 0.0838(5) 0.0816(11) 0.3444(9) 0.104(6) Uani 1 1 d . . . H12A H 0.0664 0.1291 0.3138 0.156 Uiso 1 1 calc R A . H12B H 0.0845 0.0900 0.4005 0.156 Uiso 1 1 calc R . . H12C H 0.0735 0.0191 0.3277 0.156 Uiso 1 1 calc R . . C13 C 0.2018(4) 0.2220(7) 0.3190(7) 0.050(3) Uani 1 1 d . . . H13A H 0.2165 0.1646 0.3107 0.060 Uiso 1 1 calc R A . H13B H 0.1920 0.2140 0.3679 0.060 Uiso 1 1 calc R . . C14 C 0.2292(4) 0.3040(7) 0.3273(7) 0.045(3) Uani 1 1 d . A . C15 C 0.2661(3) 0.3060(8) 0.3797(7) 0.053(3) Uani 1 1 d . . . H15A H 0.2748 0.2549 0.4142 0.063 Uiso 1 1 calc R A . C16 C 0.2898(4) 0.3833(8) 0.3808(7) 0.060(3) Uani 1 1 d . A . H16A H 0.3158 0.3845 0.4146 0.071 Uiso 1 1 calc R . . C17 C 0.2766(4) 0.4596(8) 0.3332(7) 0.051(3) Uani 1 1 d . . . H17A H 0.2929 0.5136 0.3344 0.061 Uiso 1 1 calc R A . C18 C 0.2383(3) 0.4550(7) 0.2830(6) 0.040(3) Uani 1 1 d . A . C19 C 0.2212(4) 0.5335(7) 0.2293(6) 0.053(3) Uani 1 1 d . . . H19A H 0.2162 0.5879 0.2610 0.063 Uiso 1 1 calc R A . H19B H 0.2408 0.5529 0.1983 0.063 Uiso 1 1 calc R . . C20 C 0.1653(3) 0.5782(7) 0.1214(6) 0.043(3) Uani 1 1 d . . . C21 C 0.1472(4) 0.6549(7) 0.1487(7) 0.054(3) Uani 1 1 d . A . C22 C 0.1287(4) 0.7257(9) 0.0965(7) 0.062(4) Uani 1 1 d . . . H22A H 0.1150 0.7763 0.1141 0.074 Uiso 1 1 calc R A . C23 C 0.1313(4) 0.7182(9) 0.0182(8) 0.064(4) Uani 1 1 d . A . H23A H 0.1198 0.7658 -0.0179 0.077 Uiso 1 1 calc R . . C24 C 0.1506(4) 0.6420(10) -0.0090(7) 0.066(4) Uani 1 1 d . . . H24A H 0.1518 0.6388 -0.0629 0.080 Uiso 1 1 calc R A . C25 C 0.1675(3) 0.5734(8) 0.0412(6) 0.045(3) Uani 1 1 d . A . C26 C 0.1430(5) 0.6662(9) 0.2329(8) 0.075(4) Uani 1 1 d . . . H26A H 0.1560 0.6103 0.2625 0.090 Uiso 1 1 calc R A . C27 C 0.0985(5) 0.6671(12) 0.2417(11) 0.131(7) Uani 1 1 d . A . H27A H 0.0847 0.6112 0.2166 0.196 Uiso 1 1 calc R . . H27B H 0.0850 0.7232 0.2164 0.196 Uiso 1 1 calc R . . H27C H 0.0980 0.6673 0.2977 0.196 Uiso 1 1 calc R . . C28 C 0.1656(6) 0.7530(10) 0.2734(7) 0.110(7) Uani 1 1 d . A . H28A H 0.1626 0.7565 0.3280 0.165 Uiso 1 1 calc R . . H28B H 0.1543 0.8096 0.2450 0.165 Uiso 1 1 calc R . . H28C H 0.1940 0.7480 0.2727 0.165 Uiso 1 1 calc R . . C29 C 0.1895(4) 0.4922(8) 0.0117(7) 0.060(4) Uani 1 1 d . . . H29A H 0.1849 0.4349 0.0415 0.072 Uiso 1 1 calc R A . C30 C 0.2343(5) 0.5085(11) 0.0273(9) 0.097(5) Uani 1 1 d . A . H30A H 0.2447 0.5214 0.0834 0.145 Uiso 1 1 calc R . . H30B H 0.2398 0.5621 -0.0038 0.145 Uiso 1 1 calc R . . H30C H 0.2474 0.4526 0.0123 0.145 Uiso 1 1 calc R . . C31 C 0.1742(5) 0.4710(9) -0.0775(7) 0.090(5) Uani 1 1 d . A . H31A H 0.1892 0.4181 -0.0922 0.135 Uiso 1 1 calc R . . H31B H 0.1782 0.5262 -0.1083 0.135 Uiso 1 1 calc R . . H31C H 0.1457 0.4554 -0.0883 0.135 Uiso 1 1 calc R . . C32 C 0.0876(4) 0.3880(9) 0.0483(7) 0.066(4) Uani 1 1 d . A . H32A H 0.0600 0.3977 0.0199 0.098 Uiso 1 1 d R . . H32B H 0.1045 0.4364 0.0364 0.098 Uiso 1 1 d R . . H32C H 0.0968 0.3281 0.0331 0.098 Uiso 1 1 d R . . C33 C 0.0916(4) 0.3887(9) 0.2490(7) 0.072(4) Uani 1 1 d . A . H33A H 0.0652 0.3994 0.2576 0.108 Uiso 1 1 d R . . H33B H 0.1015 0.3298 0.2709 0.108 Uiso 1 1 d R . . H33C H 0.1091 0.4381 0.2741 0.108 Uiso 1 1 d R . . Li1 Li 0.0539(6) 0.3770(15) 0.1412(10) 0.067(6) Uani 0.587(10) 1 d PD A 1 O1 O 0.0012(4) 0.4482(8) 0.1317(10) 0.097(5) Uiso 0.587(10) 1 d PD A 1 O2 O 0.0161(3) 0.2700(7) 0.1055(11) 0.076(4) Uiso 0.587(10) 1 d PD A 1 C34 C -0.0028(6) 0.5466(13) 0.1337(19) 0.124(10) Uiso 0.587(10) 1 d PD A 1 H34A H -0.0292 0.5649 0.1025 0.185 Uiso 0.587(10) 1 calc PR A 1 H34B H 0.0181 0.5760 0.1116 0.185 Uiso 0.587(10) 1 calc PR A 1 H34C H 0.0000 0.5672 0.1883 0.185 Uiso 0.587(10) 1 calc PR A 1 C35 C -0.0294(5) 0.3907(10) 0.0802(14) 0.073(6) Uiso 0.587(10) 1 d PD A 1 H35A H -0.0246 0.3875 0.0263 0.088 Uiso 0.587(10) 1 calc PR A 1 H35B H -0.0566 0.4161 0.0775 0.088 Uiso 0.587(10) 1 calc PR A 1 C36 C -0.0245(5) 0.2957(13) 0.1191(12) 0.087(7) Uiso 0.587(10) 1 d PD A 1 H36A H -0.0244 0.2996 0.1759 0.104 Uiso 0.587(10) 1 calc PR A 1 H36B H -0.0455 0.2513 0.0929 0.104 Uiso 0.587(10) 1 calc PR A 1 C37 C 0.0245(6) 0.1755(11) 0.1404(13) 0.082(7) Uiso 0.587(10) 1 d PD A 1 H37A H 0.0034 0.1322 0.1148 0.123 Uiso 0.587(10) 1 calc PR A 1 H37B H 0.0252 0.1783 0.1969 0.123 Uiso 0.587(10) 1 calc PR A 1 H37C H 0.0505 0.1536 0.1326 0.123 Uiso 0.587(10) 1 calc PR A 1 Li1' Li 0.0539(6) 0.3770(15) 0.1412(10) 0.067(6) Uani 0.413(10) 1 d PD A 2 O1' O 0.0032(4) 0.4527(10) 0.0966(12) 0.097(5) Uiso 0.413(10) 1 d PD A 2 O2' O 0.0142(4) 0.2715(8) 0.1284(14) 0.076(4) Uiso 0.413(10) 1 d PD A 2 C34' C 0.0004(7) 0.5514(14) 0.097(2) 0.124(10) Uiso 0.413(10) 1 d PD A 2 H34D H -0.0277 0.5698 0.0923 0.185 Uiso 0.413(10) 1 calc PR A 2 H34E H 0.0103 0.5773 0.0532 0.185 Uiso 0.413(10) 1 calc PR A 2 H34F H 0.0165 0.5756 0.1470 0.185 Uiso 0.413(10) 1 calc PR A 2 C35' C -0.0302(5) 0.3944(14) 0.1090(19) 0.073(6) Uiso 0.413(10) 1 d PD A 2 H35C H -0.0563 0.4221 0.0829 0.088 Uiso 0.413(10) 1 calc PR A 2 H35D H -0.0293 0.3867 0.1658 0.088 Uiso 0.413(10) 1 calc PR A 2 C36' C -0.0237(6) 0.3020(15) 0.0718(15) 0.087(7) Uiso 0.413(10) 1 d PD A 2 H36C H -0.0460 0.2578 0.0712 0.104 Uiso 0.413(10) 1 calc PR A 2 H36D H -0.0196 0.3100 0.0177 0.104 Uiso 0.413(10) 1 calc PR A 2 C37' C 0.0237(6) 0.1786(11) 0.0995(16) 0.082(7) Uiso 0.413(10) 1 d PD A 2 H37D H 0.0014 0.1356 0.0989 0.123 Uiso 0.413(10) 1 calc PR A 2 H37E H 0.0480 0.1538 0.1344 0.123 Uiso 0.413(10) 1 calc PR A 2 H37F H 0.0281 0.1849 0.0460 0.123 Uiso 0.413(10) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Th1 0.0481(3) 0.0400(2) 0.0375(2) 0.0024(2) 0.00174(17) 0.0008(3) N1 0.056(7) 0.030(5) 0.043(6) 0.005(4) -0.003(5) -0.007(5) N2 0.045(6) 0.044(6) 0.036(5) -0.008(4) 0.008(4) -0.005(5) N3 0.046(6) 0.036(5) 0.045(6) 0.017(4) -0.002(5) 0.012(5) C1 0.077(10) 0.033(8) 0.054(8) 0.000(6) 0.009(7) 0.007(6) C2 0.046(8) 0.039(8) 0.053(8) -0.003(6) 0.030(6) 0.006(6) C3 0.075(10) 0.039(7) 0.043(7) -0.010(6) -0.001(7) 0.007(7) C4 0.067(9) 0.037(7) 0.065(10) -0.002(6) 0.003(7) 0.006(6) C5 0.067(9) 0.041(7) 0.061(9) -0.004(6) -0.004(7) -0.009(6) C6 0.063(9) 0.030(6) 0.051(8) 0.005(6) 0.008(6) 0.005(6) C7 0.058(9) 0.059(8) 0.035(7) 0.009(6) 0.012(6) -0.001(7) C8 0.160(16) 0.048(9) 0.062(10) -0.010(7) 0.027(10) -0.004(9) C9 0.099(13) 0.053(8) 0.075(10) -0.004(7) 0.042(9) -0.002(8) C10 0.084(11) 0.045(7) 0.055(8) 0.003(6) 0.027(7) -0.011(7) C11 0.139(15) 0.069(10) 0.071(10) 0.021(8) 0.018(10) 0.014(10) C12 0.123(15) 0.082(11) 0.122(15) -0.019(10) 0.061(12) -0.033(11) C13 0.061(9) 0.042(7) 0.049(8) -0.001(6) 0.014(7) 0.009(6) C14 0.053(8) 0.029(6) 0.049(7) -0.007(5) 0.005(6) 0.026(6) C15 0.047(8) 0.036(7) 0.068(9) 0.001(6) -0.003(7) 0.000(6) C16 0.048(8) 0.060(9) 0.062(8) -0.016(7) -0.007(6) -0.001(6) C17 0.051(9) 0.038(7) 0.064(9) 0.007(6) 0.015(7) 0.003(6) C18 0.028(7) 0.039(7) 0.054(8) -0.003(6) 0.009(6) 0.011(5) C19 0.075(10) 0.039(7) 0.040(7) 0.011(5) 0.003(7) -0.010(6) C20 0.049(8) 0.031(7) 0.044(7) 0.003(5) 0.003(6) -0.009(6) C21 0.074(9) 0.033(8) 0.054(8) 0.007(5) 0.011(7) -0.012(6) C22 0.068(10) 0.063(9) 0.052(9) 0.010(7) 0.009(7) -0.003(7) C23 0.066(10) 0.045(8) 0.062(10) 0.014(7) -0.026(7) -0.014(7) C24 0.082(10) 0.063(9) 0.048(8) 0.014(8) 0.002(7) -0.018(9) C25 0.054(8) 0.046(7) 0.030(7) 0.009(6) -0.004(6) -0.007(6) C26 0.100(13) 0.057(10) 0.070(10) 0.007(7) 0.026(9) 0.015(8) C27 0.132(17) 0.142(16) 0.138(17) 0.041(13) 0.074(14) 0.063(13) C28 0.23(2) 0.073(11) 0.033(8) -0.006(7) 0.048(11) 0.028(12) C29 0.095(12) 0.053(8) 0.036(7) 0.006(6) 0.021(7) -0.005(8) C30 0.084(13) 0.112(13) 0.093(12) -0.035(10) 0.019(10) 0.019(10) C31 0.144(15) 0.073(10) 0.053(9) -0.001(7) 0.022(9) -0.020(9) C32 0.043(8) 0.082(10) 0.070(9) 0.002(7) 0.009(7) -0.011(7) C33 0.062(9) 0.096(11) 0.058(8) -0.011(7) 0.013(7) 0.008(8) Li1 0.057(14) 0.063(15) 0.077(15) 0.004(12) 0.003(12) 0.010(11) Li1' 0.057(14) 0.063(15) 0.077(15) 0.004(12) 0.003(12) 0.010(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Th1 N1 2.304(8) . ? Th1 N3 2.346(9) . ? Th1 C7 2.565(11) . ? Th1 N2 2.617(9) . ? Th1 C33 2.633(12) . ? Th1 C32 2.686(12) . ? Th1 C1 3.049(11) . ? Th1 Li1 3.19(2) . ? Th1 H33B 2.6576 . ? N1 C1 1.437(13) . ? N1 C13 1.457(13) . ? N2 C18 1.343(12) . ? N2 C14 1.352(12) . ? N3 C20 1.448(12) . ? N3 C19 1.459(13) . ? C1 C6 1.421(15) . ? C1 C2 1.459(15) . ? C2 C3 1.419(15) . ? C2 C7 1.512(14) . ? C3 C4 1.389(15) . ? C3 H3A 0.9500 . ? C4 C5 1.373(15) . ? C4 H4A 0.9500 . ? C5 C6 1.403(15) . ? C5 H5A 0.9500 . ? C6 C10 1.536(15) . ? C7 C9 1.510(17) . ? C7 C8 1.549(15) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.535(17) . ? C10 C11 1.543(17) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.487(15) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.386(15) . ? C15 C16 1.368(15) . ? C15 H15A 0.9500 . ? C16 C17 1.383(14) . ? C16 H16A 0.9500 . ? C17 C18 1.405(15) . ? C17 H17A 0.9500 . ? C18 C19 1.495(14) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.395(15) . ? C20 C25 1.417(14) . ? C21 C22 1.412(15) . ? C21 C26 1.514(17) . ? C22 C23 1.390(16) . ? C22 H22A 0.9500 . ? C23 C24 1.410(17) . ? C23 H23A 0.9500 . ? C24 C25 1.354(15) . ? C24 H24A 0.9500 . ? C25 C29 1.532(16) . ? C26 C28 1.545(18) . ? C26 C27 1.57(2) . ? C26 H26A 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.517(17) . ? C29 C31 1.555(16) . ? C29 H29A 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 Li1 2.19(2) . ? C32 H32A 0.9744 . ? C32 H32B 0.9534 . ? C32 H32C 0.9699 . ? C33 Li1 2.04(2) . ? C33 H33A 0.9618 . ? C33 H33B 0.9539 . ? C33 H33C 0.9644 . ? Li1 O2 2.01(2) . ? Li1 O1 2.05(2) . ? Li1 H32A 2.1881 . ? Li1 H33A 2.0043 . ? O1 C34 1.413(18) . ? O1 C35 1.469(17) . ? O2 C37 1.482(17) . ? O2 C36 1.508(18) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.51(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? O1' C34' 1.414(18) . ? O1' C35' 1.469(17) . ? O2' C37' 1.482(17) . ? O2' C36' 1.508(18) . ? C34' H34D 0.9800 . ? C34' H34E 0.9800 . ? C34' H34F 0.9800 . ? C35' C36' 1.51(2) . ? C35' H35C 0.9900 . ? C35' H35D 0.9900 . ? C36' H36C 0.9900 . ? C36' H36D 0.9900 . ? C37' H37D 0.9800 . ? C37' H37E 0.9800 . ? C37' H37F 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 N1 Th1 N3 127.0(3) . . ? N1 Th1 C7 70.9(3) . . ? N3 Th1 C7 117.3(3) . . ? N1 Th1 N2 63.0(3) . . ? N3 Th1 N2 64.0(3) . . ? C7 Th1 N2 99.5(3) . . ? N1 Th1 C33 86.8(4) . . ? N3 Th1 C33 107.8(4) . . ? C7 Th1 C33 134.5(4) . . ? N2 Th1 C33 104.8(3) . . ? N1 Th1 C32 130.7(3) . . ? N3 Th1 C32 102.1(3) . . ? C7 Th1 C32 84.2(4) . . ? N2 Th1 C32 165.9(3) . . ? C33 Th1 C32 81.4(4) . . ? N1 Th1 C1 26.8(3) . . ? N3 Th1 C1 149.9(3) . . ? C7 Th1 C1 53.6(3) . . ? N2 Th1 C1 88.0(3) . . ? C33 Th1 C1 89.2(4) . . ? C32 Th1 C1 105.0(3) . . ? N1 Th1 Li1 106.8(4) . . ? N3 Th1 Li1 116.6(4) . . ? C7 Th1 Li1 109.4(5) . . ? N2 Th1 Li1 144.2(4) . . ? C33 Th1 Li1 39.5(4) . . ? C32 Th1 Li1 42.8(4) . . ? C1 Th1 Li1 92.4(4) . . ? N1 Th1 H33B 66.2 . . ? N3 Th1 H33B 121.7 . . ? C7 Th1 H33B 119.9 . . ? N2 Th1 H33B 96.4 . . ? C33 Th1 H33B 20.8 . . ? C32 Th1 H33B 93.4 . . ? C1 Th1 H33B 69.6 . . ? Li1 Th1 H33B 51.0 . . ? C1 N1 C13 119.5(9) . . ? C1 N1 Th1 106.9(7) . . ? C13 N1 Th1 130.6(7) . . ? C18 N2 C14 120.1(9) . . ? C18 N2 Th1 119.4(7) . . ? C14 N2 Th1 119.9(7) . . ? C20 N3 C19 114.7(8) . . ? C20 N3 Th1 117.1(7) . . ? C19 N3 Th1 128.1(6) . . ? C6 C1 N1 124.3(11) . . ? C6 C1 C2 119.7(11) . . ? N1 C1 C2 115.5(10) . . ? C6 C1 Th1 142.8(8) . . ? N1 C1 Th1 46.3(5) . . ? C2 C1 Th1 77.8(6) . . ? C3 C2 C1 116.8(10) . . ? C3 C2 C7 123.5(10) . . ? C1 C2 C7 119.7(10) . . ? C4 C3 C2 121.9(11) . . ? C4 C3 H3A 119.1 . . ? C2 C3 H3A 119.1 . . ? C5 C4 C3 120.7(12) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 120.8(11) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C5 C6 C1 119.6(11) . . ? C5 C6 C10 120.8(11) . . ? C1 C6 C10 119.5(10) . . ? C9 C7 C2 114.4(10) . . ? C9 C7 C8 107.7(10) . . ? C2 C7 C8 111.1(10) . . ? C9 C7 Th1 101.4(7) . . ? C2 C7 Th1 95.0(6) . . ? C8 C7 Th1 126.9(8) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C6 113.3(12) . . ? C12 C10 C11 111.0(11) . . ? C6 C10 C11 109.4(10) . . ? C12 C10 H10A 107.6 . . ? C6 C10 H10A 107.6 . . ? C11 C10 H10A 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 110.2(9) . . ? N1 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? N1 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N2 C14 C15 121.4(11) . . ? N2 C14 C13 115.6(10) . . ? C15 C14 C13 122.9(10) . . ? C16 C15 C14 118.5(11) . . ? C16 C15 H15A 120.7 . . ? C14 C15 H15A 120.7 . . ? C15 C16 C17 120.9(11) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C16 C17 C18 118.1(11) . . ? C16 C17 H17A 120.9 . . ? C18 C17 H17A 120.9 . . ? N2 C18 C17 120.8(10) . . ? N2 C18 C19 116.8(10) . . ? C17 C18 C19 122.3(10) . . ? N3 C19 C18 111.2(9) . . ? N3 C19 H19A 109.4 . . ? C18 C19 H19A 109.4 . . ? N3 C19 H19B 109.4 . . ? C18 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C21 C20 C25 120.0(10) . . ? C21 C20 N3 120.0(10) . . ? C25 C20 N3 119.9(10) . . ? C20 C21 C22 120.8(11) . . ? C20 C21 C26 124.1(10) . . ? C22 C21 C26 114.9(11) . . ? C23 C22 C21 117.3(12) . . ? C23 C22 H22A 121.3 . . ? C21 C22 H22A 121.3 . . ? C22 C23 C24 121.8(12) . . ? C22 C23 H23A 119.1 . . ? C24 C23 H23A 119.1 . . ? C25 C24 C23 120.4(12) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C24 C25 C20 119.5(11) . . ? C24 C25 C29 120.1(11) . . ? C20 C25 C29 120.3(10) . . ? C21 C26 C28 112.4(11) . . ? C21 C26 C27 113.6(13) . . ? C28 C26 C27 110.3(13) . . ? C21 C26 H26A 106.7 . . ? C28 C26 H26A 106.7 . . ? C27 C26 H26A 106.7 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C25 112.2(10) . . ? C30 C29 C31 108.0(11) . . ? C25 C29 C31 113.7(11) . . ? C30 C29 H29A 107.6 . . ? C25 C29 H29A 107.6 . . ? C31 C29 H29A 107.6 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Li1 C32 Th1 80.9(6) . . ? Li1 C32 H32A 76.9 . . ? Th1 C32 H32A 157.7 . . ? Li1 C32 H32B 131.2 . . ? Th1 C32 H32B 82.2 . . ? H32A C32 H32B 110.8 . . ? Li1 C32 H32C 113.3 . . ? Th1 C32 H32C 82.1 . . ? H32A C32 H32C 109.0 . . ? H32B C32 H32C 109.2 . . ? Li1 C33 Th1 85.1(7) . . ? Li1 C33 H33A 74.5 . . ? Th1 C33 H33A 159.3 . . ? Li1 C33 H33B 113.0 . . ? Th1 C33 H33B 81.1 . . ? H33A C33 H33B 109.8 . . ? Li1 C33 H33C 132.9 . . ? Th1 C33 H33C 82.4 . . ? H33A C33 H33C 108.9 . . ? H33B C33 H33C 109.6 . . ? O2 Li1 C33 125.4(11) . . ? O2 Li1 O1 81.8(9) . . ? C33 Li1 O1 113.6(10) . . ? O2 Li1 C32 103.6(10) . . ? C33 Li1 C32 110.2(11) . . ? O1 Li1 C32 120.3(10) . . ? O2 Li1 Th1 124.9(9) . . ? C33 Li1 Th1 55.4(6) . . ? O1 Li1 Th1 153.2(10) . . ? C32 Li1 Th1 56.3(6) . . ? O2 Li1 H32A 89.9 . . ? C33 Li1 H32A 134.6 . . ? O1 Li1 H32A 97.3 . . ? C32 Li1 H32A 25.7 . . ? Th1 Li1 H32A 82.0 . . ? O2 Li1 H33A 113.6 . . ? C33 Li1 H33A 27.5 . . ? O1 Li1 H33A 88.2 . . ? C32 Li1 H33A 136.1 . . ? Th1 Li1 H33A 82.9 . . ? H32A Li1 H33A 156.5 . . ? C34 O1 C35 120.8(15) . . ? C34 O1 Li1 125.5(13) . . ? C35 O1 Li1 105.4(11) . . ? C37 O2 C36 105.0(13) . . ? C37 O2 Li1 120.9(11) . . ? C36 O2 Li1 108.6(11) . . ? O1 C34 H34A 109.5 . . ? O1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O1 C35 C36 103.6(16) . . ? O1 C35 H35A 111.0 . . ? C36 C35 H35A 111.0 . . ? O1 C35 H35B 111.0 . . ? C36 C35 H35B 111.0 . . ? H35A C35 H35B 109.0 . . ? O2 C36 C35 99.3(14) . . ? O2 C36 H36A 111.9 . . ? C35 C36 H36A 111.9 . . ? O2 C36 H36B 111.9 . . ? C35 C36 H36B 111.9 . . ? H36A C36 H36B 109.6 . . ? O2 C37 H37A 109.5 . . ? O2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34' O1' C35' 120.5(15) . . ? C37' O2' C36' 105.0(13) . . ? O1' C34' H34D 109.5 . . ? O1' C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? O1' C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? O1' C35' C36' 103.7(16) . . ? O1' C35' H35C 111.0 . . ? C36' C35' H35C 111.0 . . ? O1' C35' H35D 111.0 . . ? C36' C35' H35D 111.0 . . ? H35C C35' H35D 109.0 . . ? O2' C36' C35' 99.2(14) . . ? O2' C36' H36C 111.9 . . ? C35' C36' H36C 111.9 . . ? O2' C36' H36D 111.9 . . ? C35' C36' H36D 111.9 . . ? H36C C36' H36D 109.6 . . ? O2' C37' H37D 109.5 . . ? O2' C37' H37E 109.5 . . ? H37D C37' H37E 109.5 . . ? O2' C37' H37F 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Th1 N1 C1 -155.5(7) . . . . ? C7 Th1 N1 C1 -45.2(7) . . . . ? N2 Th1 N1 C1 -157.1(8) . . . . ? C33 Th1 N1 C1 94.5(8) . . . . ? C32 Th1 N1 C1 18.8(9) . . . . ? Li1 Th1 N1 C1 60.1(8) . . . . ? N3 Th1 N1 C13 4.2(11) . . . . ? C7 Th1 N1 C13 114.5(10) . . . . ? N2 Th1 N1 C13 2.6(8) . . . . ? C33 Th1 N1 C13 -105.8(9) . . . . ? C32 Th1 N1 C13 178.5(8) . . . . ? C1 Th1 N1 C13 159.7(14) . . . . ? Li1 Th1 N1 C13 -140.2(9) . . . . ? N1 Th1 N2 C18 174.4(8) . . . . ? N3 Th1 N2 C18 -4.2(7) . . . . ? C7 Th1 N2 C18 111.7(7) . . . . ? C33 Th1 N2 C18 -107.1(8) . . . . ? C32 Th1 N2 C18 7.1(16) . . . . ? C1 Th1 N2 C18 164.3(7) . . . . ? Li1 Th1 N2 C18 -104.3(10) . . . . ? N1 Th1 N2 C14 2.9(7) . . . . ? N3 Th1 N2 C14 -175.7(8) . . . . ? C7 Th1 N2 C14 -59.8(8) . . . . ? C33 Th1 N2 C14 81.4(8) . . . . ? C32 Th1 N2 C14 -164.3(12) . . . . ? C1 Th1 N2 C14 -7.2(7) . . . . ? Li1 Th1 N2 C14 84.2(10) . . . . ? N1 Th1 N3 C20 -177.9(7) . . . . ? C7 Th1 N3 C20 96.2(8) . . . . ? N2 Th1 N3 C20 -176.3(8) . . . . ? C33 Th1 N3 C20 -78.2(8) . . . . ? C32 Th1 N3 C20 6.5(8) . . . . ? C1 Th1 N3 C20 160.2(7) . . . . ? Li1 Th1 N3 C20 -36.4(9) . . . . ? N1 Th1 N3 C19 -2.0(10) . . . . ? C7 Th1 N3 C19 -87.8(9) . . . . ? N2 Th1 N3 C19 -0.4(8) . . . . ? C33 Th1 N3 C19 97.7(9) . . . . ? C32 Th1 N3 C19 -177.6(9) . . . . ? C1 Th1 N3 C19 -23.8(12) . . . . ? Li1 Th1 N3 C19 139.5(9) . . . . ? C13 N1 C1 C6 64.6(15) . . . . ? Th1 N1 C1 C6 -133.0(10) . . . . ? C13 N1 C1 C2 -123.6(11) . . . . ? Th1 N1 C1 C2 38.8(11) . . . . ? C13 N1 C1 Th1 -162.4(12) . . . . ? N1 Th1 C1 C6 91.7(16) . . . . ? N3 Th1 C1 C6 133.0(13) . . . . ? C7 Th1 C1 C6 -144.6(16) . . . . ? N2 Th1 C1 C6 112.0(14) . . . . ? C33 Th1 C1 C6 7.2(14) . . . . ? C32 Th1 C1 C6 -73.6(14) . . . . ? Li1 Th1 C1 C6 -32.1(14) . . . . ? N3 Th1 C1 N1 41.3(11) . . . . ? C7 Th1 C1 N1 123.7(9) . . . . ? N2 Th1 C1 N1 20.3(7) . . . . ? C33 Th1 C1 N1 -84.5(8) . . . . ? C32 Th1 C1 N1 -165.3(7) . . . . ? Li1 Th1 C1 N1 -123.8(8) . . . . ? N1 Th1 C1 C2 -144.7(11) . . . . ? N3 Th1 C1 C2 -103.4(8) . . . . ? C7 Th1 C1 C2 -21.0(6) . . . . ? N2 Th1 C1 C2 -124.4(7) . . . . ? C33 Th1 C1 C2 130.8(7) . . . . ? C32 Th1 C1 C2 50.0(7) . . . . ? Li1 Th1 C1 C2 91.5(7) . . . . ? C6 C1 C2 C3 -0.8(16) . . . . ? N1 C1 C2 C3 -173.0(10) . . . . ? Th1 C1 C2 C3 -145.4(9) . . . . ? C6 C1 C2 C7 178.9(10) . . . . ? N1 C1 C2 C7 6.7(15) . . . . ? Th1 C1 C2 C7 34.3(9) . . . . ? C1 C2 C3 C4 -1.9(17) . . . . ? C7 C2 C3 C4 178.4(11) . . . . ? C2 C3 C4 C5 0.3(18) . . . . ? C3 C4 C5 C6 4.3(19) . . . . ? C4 C5 C6 C1 -7.0(18) . . . . ? C4 C5 C6 C10 172.1(11) . . . . ? N1 C1 C6 C5 176.6(10) . . . . ? C2 C1 C6 C5 5.2(17) . . . . ? Th1 C1 C6 C5 115.6(13) . . . . ? N1 C1 C6 C10 -2.5(17) . . . . ? C2 C1 C6 C10 -173.9(10) . . . . ? Th1 C1 C6 C10 -63.5(18) . . . . ? C3 C2 C7 C9 -116.5(12) . . . . ? C1 C2 C7 C9 63.8(13) . . . . ? C3 C2 C7 C8 5.7(16) . . . . ? C1 C2 C7 C8 -173.9(10) . . . . ? C3 C2 C7 Th1 138.6(9) . . . . ? C1 C2 C7 Th1 -41.1(11) . . . . ? N1 Th1 C7 C9 -72.9(7) . . . . ? N3 Th1 C7 C9 49.6(8) . . . . ? N2 Th1 C7 C9 -15.9(7) . . . . ? C33 Th1 C7 C9 -137.7(7) . . . . ? C32 Th1 C7 C9 150.3(7) . . . . ? C1 Th1 C7 C9 -96.3(8) . . . . ? Li1 Th1 C7 C9 -174.5(7) . . . . ? N1 Th1 C7 C2 43.2(7) . . . . ? N3 Th1 C7 C2 165.8(6) . . . . ? N2 Th1 C7 C2 100.2(7) . . . . ? C33 Th1 C7 C2 -21.6(9) . . . . ? C32 Th1 C7 C2 -93.5(7) . . . . ? C1 Th1 C7 C2 19.8(6) . . . . ? Li1 Th1 C7 C2 -58.4(8) . . . . ? N1 Th1 C7 C8 164.4(12) . . . . ? N3 Th1 C7 C8 -73.0(11) . . . . ? N2 Th1 C7 C8 -138.6(11) . . . . ? C33 Th1 C7 C8 99.6(11) . . . . ? C32 Th1 C7 C8 27.7(11) . . . . ? C1 Th1 C7 C8 141.0(12) . . . . ? Li1 Th1 C7 C8 62.8(12) . . . . ? C5 C6 C10 C12 -48.7(16) . . . . ? C1 C6 C10 C12 130.4(12) . . . . ? C5 C6 C10 C11 75.8(15) . . . . ? C1 C6 C10 C11 -105.1(13) . . . . ? C1 N1 C13 C14 150.6(10) . . . . ? Th1 N1 C13 C14 -6.9(13) . . . . ? C18 N2 C14 C15 2.2(15) . . . . ? Th1 N2 C14 C15 173.6(8) . . . . ? C18 N2 C14 C13 -178.8(9) . . . . ? Th1 N2 C14 C13 -7.4(12) . . . . ? N1 C13 C14 N2 8.5(13) . . . . ? N1 C13 C14 C15 -172.5(10) . . . . ? N2 C14 C15 C16 -3.6(17) . . . . ? C13 C14 C15 C16 177.4(10) . . . . ? C14 C15 C16 C17 3.0(18) . . . . ? C15 C16 C17 C18 -0.9(17) . . . . ? C14 N2 C18 C17 0.0(15) . . . . ? Th1 N2 C18 C17 -171.5(8) . . . . ? C14 N2 C18 C19 179.4(9) . . . . ? Th1 N2 C18 C19 7.9(12) . . . . ? C16 C17 C18 N2 -0.6(16) . . . . ? C16 C17 C18 C19 -180.0(10) . . . . ? C20 N3 C19 C18 -179.8(9) . . . . ? Th1 N3 C19 C18 4.2(14) . . . . ? N2 C18 C19 N3 -7.6(14) . . . . ? C17 C18 C19 N3 171.8(10) . . . . ? C19 N3 C20 C21 -71.8(13) . . . . ? Th1 N3 C20 C21 104.7(10) . . . . ? C19 N3 C20 C25 105.0(12) . . . . ? Th1 N3 C20 C25 -78.6(11) . . . . ? C25 C20 C21 C22 3.9(17) . . . . ? N3 C20 C21 C22 -179.4(10) . . . . ? C25 C20 C21 C26 179.3(12) . . . . ? N3 C20 C21 C26 -3.9(18) . . . . ? C20 C21 C22 C23 -3.6(18) . . . . ? C26 C21 C22 C23 -179.4(11) . . . . ? C21 C22 C23 C24 1.8(18) . . . . ? C22 C23 C24 C25 -0.2(19) . . . . ? C23 C24 C25 C20 0.5(18) . . . . ? C23 C24 C25 C29 -178.3(11) . . . . ? C21 C20 C25 C24 -2.3(17) . . . . ? N3 C20 C25 C24 -179.0(10) . . . . ? C21 C20 C25 C29 176.5(11) . . . . ? N3 C20 C25 C29 -0.3(16) . . . . ? C20 C21 C26 C28 117.8(13) . . . . ? C22 C21 C26 C28 -66.5(16) . . . . ? C20 C21 C26 C27 -116.0(14) . . . . ? C22 C21 C26 C27 59.7(15) . . . . ? C24 C25 C29 C30 96.0(14) . . . . ? C20 C25 C29 C30 -82.8(14) . . . . ? C24 C25 C29 C31 -26.9(16) . . . . ? C20 C25 C29 C31 154.3(11) . . . . ? N1 Th1 C32 Li1 68.3(8) . . . . ? N3 Th1 C32 Li1 -116.3(6) . . . . ? C7 Th1 C32 Li1 126.9(7) . . . . ? N2 Th1 C32 Li1 -126.7(12) . . . . ? C33 Th1 C32 Li1 -9.8(7) . . . . ? C1 Th1 C32 Li1 77.0(7) . . . . ? N1 Th1 C33 Li1 -121.6(7) . . . . ? N3 Th1 C33 Li1 110.5(7) . . . . ? C7 Th1 C33 Li1 -62.6(9) . . . . ? N2 Th1 C33 Li1 177.4(7) . . . . ? C32 Th1 C33 Li1 10.4(7) . . . . ? C1 Th1 C33 Li1 -94.8(7) . . . . ? Th1 C33 Li1 O2 111.2(13) . . . . ? Th1 C33 Li1 O1 -151.9(10) . . . . ? Th1 C33 Li1 C32 -13.5(9) . . . . ? Th1 C32 Li1 O2 -123.1(9) . . . . ? Th1 C32 Li1 C33 13.4(9) . . . . ? Th1 C32 Li1 O1 148.5(12) . . . . ? N1 Th1 Li1 O2 -49.5(11) . . . . ? N3 Th1 Li1 O2 161.8(10) . . . . ? C7 Th1 Li1 O2 25.6(12) . . . . ? N2 Th1 Li1 O2 -116.4(11) . . . . ? C33 Th1 Li1 O2 -112.2(13) . . . . ? C32 Th1 Li1 O2 83.1(11) . . . . ? C1 Th1 Li1 O2 -26.5(11) . . . . ? N1 Th1 Li1 C33 62.7(7) . . . . ? N3 Th1 Li1 C33 -86.0(7) . . . . ? C7 Th1 Li1 C33 137.8(6) . . . . ? N2 Th1 Li1 C33 -4.3(11) . . . . ? C32 Th1 Li1 C33 -164.7(10) . . . . ? C1 Th1 Li1 C33 85.7(7) . . . . ? N1 Th1 Li1 O1 135.9(18) . . . . ? N3 Th1 Li1 O1 -13(2) . . . . ? C7 Th1 Li1 O1 -149.0(18) . . . . ? N2 Th1 Li1 O1 69(2) . . . . ? C33 Th1 Li1 O1 73.2(18) . . . . ? C32 Th1 Li1 O1 -92(2) . . . . ? C1 Th1 Li1 O1 158.9(19) . . . . ? N1 Th1 Li1 C32 -132.6(6) . . . . ? N3 Th1 Li1 C32 78.7(6) . . . . ? C7 Th1 Li1 C32 -57.5(7) . . . . ? N2 Th1 Li1 C32 160.4(5) . . . . ? C33 Th1 Li1 C32 164.7(10) . . . . ? C1 Th1 Li1 C32 -109.6(6) . . . . ? O2 Li1 O1 C34 -168(2) . . . . ? C33 Li1 O1 C34 67(2) . . . . ? C32 Li1 O1 C34 -67(2) . . . . ? Th1 Li1 O1 C34 8(3) . . . . ? O2 Li1 O1 C35 -19.7(13) . . . . ? C33 Li1 O1 C35 -144.9(15) . . . . ? C32 Li1 O1 C35 81.4(17) . . . . ? Th1 Li1 O1 C35 155.9(19) . . . . ? C33 Li1 O2 C37 -26(2) . . . . ? O1 Li1 O2 C37 -139.5(15) . . . . ? C32 Li1 O2 C37 101.2(16) . . . . ? Th1 Li1 O2 C37 43(2) . . . . ? C33 Li1 O2 C36 95.0(17) . . . . ? O1 Li1 O2 C36 -18.1(12) . . . . ? C32 Li1 O2 C36 -137.5(13) . . . . ? Th1 Li1 O2 C36 164.3(12) . . . . ? C34 O1 C35 C36 -156.3(19) . . . . ? Li1 O1 C35 C36 53.8(16) . . . . ? C37 O2 C36 C35 -179.1(15) . . . . ? Li1 O2 C36 C35 50.2(16) . . . . ? O1 C35 C36 O2 -67.7(17) . . . . ? C34' O1' C35' C36' 157.4(19) . . . . ? C37' O2' C36' C35' 178.6(15) . . . . ? O1' C35' C36' O2' 67.8(17) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.151 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.160 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.005 529.0 184.7 2 0.500 0.500 0.223 529.0 184.6 _platon_squeeze_details ; One disordered molecule of hexane was removed via squeeze. ; _vrf_PLAT390_cruz50 ; PROBLEM: Deviating Methyl C32 X-C-H Bond Angle ...... 158.00 Deg. RESPONSE: These methyl groups are 5-coordinate since they bridge between thorium and lithium. ; _vrf_CHEMW03_cruz50 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10 RESPONSE: One molecule of highly disordered hexane was removed using the SQUEEZE routine. The atom site* data does not include this hexane, while the overall compound formula and the expected molecular weight does. ; _vrf_PLAT043_cruz50 ; PROBLEM: Check Reported Molecular Weight ................ 900.02 RESPONSE: One molecule of highly disordered hexane was removed using the SQUEEZE routine. The atom site* data does not include this hexane, while the overall compound formula and the expected molecular weight does. ; # end Validation Reply Form