# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Moris Eisen' 'Sinai Aharonovich' 'Mark Botoshansky' 'Elena Rabinovich' _publ_contact_author_name 'Moris Eisen' _publ_contact_author_email CHMORIS@TX.TECHNION.AC.IL _publ_section_title ; Thorium 2-Pyridylamidinates: Synthesis, Structure and Catalytic Activity Towards the Cyclo-oligomerization of ?-Caprolactone. ; # Attachment 'Th amidinates.cif' data_complex2 _database_code_depnum_ccdc_archive 'CCDC 761284' #TrackingRef 'Th amidinates.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common complex2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H70 Cl3 Li N8 Si4 Th' _chemical_formula_weight 1084.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.333(4) _cell_length_b 11.771(2) _cell_length_c 21.970(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.38(3) _cell_angle_gamma 90.00 _cell_volume 5188.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 240(1) _cell_measurement_reflns_used 26395 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 25.32 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 3.154 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.69623 _exptl_absorpt_correction_T_max 0.90695 _exptl_absorpt_process_details ; 'PLATON (Spek, A.L. 1995)' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method phi-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21938 _diffrn_reflns_av_R_equivalents 0.1000 _diffrn_reflns_av_sigmaI/netI 0.1162 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.32 _reflns_number_total 9186 _reflns_number_gt 5360 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2006)' _computing_cell_refinement 'DENZO HKL2000 (Otwinowski & Minor 1997)' _computing_data_reduction 'DENZO HKL2000 (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'TEXSAN (MSC, 1999)' _computing_publication_material ? _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^)+(0.0698P)^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 SHELXL _refine_ls_extinction_coef 0.0018(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9186 _refine_ls_number_parameters 429 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1417 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.1808 _refine_ls_wR_factor_gt 0.1638 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 0.060 _refine_ls_shift/su_mean 0.002 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 0.22386(2) 0.50743(3) 0.394276(18) 0.04407(19) Uani 1 1 d . . . Cl1 Cl 0.3253(2) 0.3956(3) 0.35681(18) 0.0751(11) Uani 1 1 d . . . Cl2 Cl 0.1075(2) 0.6202(3) 0.33820(18) 0.0753(11) Uani 1 1 d . . . Cl3 Cl 0.1524(2) 0.3468(3) 0.31470(16) 0.0725(11) Uani 1 1 d . . . Si1 Si 0.10464(19) 0.3306(3) 0.48597(17) 0.0557(9) Uani 1 1 d . . . Si2 Si 0.3690(2) 0.4703(4) 0.5330(2) 0.0786(13) Uani 1 1 d . . . Si3 Si 0.1955(2) 0.7693(3) 0.50212(16) 0.0524(9) Uani 1 1 d . . . Si4 Si 0.3188(2) 0.7060(3) 0.29523(17) 0.0627(11) Uani 1 1 d . . . N1 N 0.1774(5) 0.4006(7) 0.4761(4) 0.040(2) Uani 1 1 d . . . N2 N 0.2873(5) 0.4564(8) 0.4956(4) 0.048(2) Uani 1 1 d . . . N3 N 0.2291(5) 0.7000(7) 0.4437(4) 0.043(2) Uani 1 1 d . . . N4 N 0.2789(5) 0.6748(7) 0.3578(4) 0.048(2) Uani 1 1 d . . . N5 N 0.0638(6) 0.4872(9) 0.1776(5) 0.066(3) Uani 1 1 d D . . N6 N -0.0421(6) 0.4744(9) 0.2496(5) 0.064(3) Uani 1 1 d D . . Li1 Li 0.0636(13) 0.472(2) 0.2698(10) 0.075(7) Uani 1 1 d . . . C1 C 0.2367(7) 0.3995(8) 0.5114(6) 0.053(3) Uani 1 1 d . . . C2 C 0.2473(6) 0.3330(10) 0.5721(5) 0.051(3) Uani 1 1 d . . . N31 N 0.2393(7) 0.3906(9) 0.6233(6) 0.083(4) Uani 1 1 d . . . H31 H 0.2280 0.4611 0.6215 0.100 Uiso 1 1 calc R . . C4 C 0.2496(8) 0.3353(13) 0.6767(6) 0.081(5) Uani 1 1 d . . . H4 H 0.2431 0.3740 0.7122 0.097 Uiso 1 1 calc R . . C5 C 0.2690(8) 0.2246(13) 0.6819(8) 0.079(5) Uani 1 1 d . . . H5 H 0.2762 0.1889 0.7201 0.095 Uiso 1 1 calc R . . C6 C 0.2774(7) 0.1692(12) 0.6320(7) 0.074(4) Uani 1 1 d . . . H6 H 0.2902 0.0933 0.6345 0.089 Uiso 1 1 calc R . . C7 C 0.2670(6) 0.2242(9) 0.5754(6) 0.052(3) Uani 1 1 d . . . H7 H 0.2736 0.1858 0.5399 0.063 Uiso 1 1 calc R . . C8 C 0.0377(7) 0.3802(17) 0.4256(8) 0.123(8) Uani 1 1 d . . . H8A H 0.0491 0.3635 0.3858 0.184 Uiso 1 1 calc R . . H8B H 0.0321 0.4607 0.4295 0.184 Uiso 1 1 calc R . . H8C H -0.0031 0.3422 0.4298 0.184 Uiso 1 1 calc R . . C9 C 0.0812(8) 0.3606(14) 0.5603(7) 0.091(5) Uani 1 1 d . . . H9A H 0.1154 0.3337 0.5924 0.136 Uiso 1 1 calc R . . H9B H 0.0399 0.3230 0.5633 0.136 Uiso 1 1 calc R . . H9C H 0.0758 0.4411 0.5647 0.136 Uiso 1 1 calc R . . C10 C 0.1113(8) 0.1764(11) 0.4753(8) 0.084(5) Uani 1 1 d . . . H10A H 0.1460 0.1465 0.5060 0.126 Uiso 1 1 calc R . . H10B H 0.1216 0.1612 0.4350 0.126 Uiso 1 1 calc R . . H10C H 0.0697 0.1409 0.4793 0.126 Uiso 1 1 calc R . . C11 C 0.4071(7) 0.5744(12) 0.4877(8) 0.086(5) Uani 1 1 d . . . H11A H 0.4064 0.5458 0.4467 0.128 Uiso 1 1 calc R . . H11B H 0.4524 0.5878 0.5068 0.128 Uiso 1 1 calc R . . H11C H 0.3825 0.6443 0.4859 0.128 Uiso 1 1 calc R . . C12 C 0.4153(9) 0.3356(16) 0.5355(13) 0.184(14) Uani 1 1 d . . . H12A H 0.3958 0.2814 0.5599 0.277 Uiso 1 1 calc R . . H12B H 0.4610 0.3484 0.5535 0.277 Uiso 1 1 calc R . . H12C H 0.4132 0.3068 0.4943 0.277 Uiso 1 1 calc R . . C13 C 0.3752(11) 0.530(3) 0.6100(10) 0.233(19) Uani 1 1 d . . . H13A H 0.3561 0.4777 0.6359 0.349 Uiso 1 1 calc R . . H13B H 0.3515 0.6006 0.6080 0.349 Uiso 1 1 calc R . . H13C H 0.4212 0.5423 0.6269 0.349 Uiso 1 1 calc R . . C14 C 0.2613(6) 0.7436(9) 0.4016(6) 0.049(3) Uani 1 1 d . . . C15 C 0.2833(7) 0.8665(9) 0.4039(6) 0.047(3) Uani 1 1 d . . . C16 C 0.3478(8) 0.8936(11) 0.4202(7) 0.069(4) Uani 1 1 d . . . H16 H 0.3802 0.8382 0.4314 0.083 Uiso 1 1 calc R . . C17 C 0.3646(9) 1.0105(13) 0.4195(8) 0.093(6) Uani 1 1 d . . . H17 H 0.4090 1.0319 0.4310 0.112 Uiso 1 1 calc R . . C18 C 0.3194(12) 1.0903(12) 0.4030(8) 0.094(6) Uani 1 1 d . . . H18 H 0.3303 1.1670 0.4036 0.112 Uiso 1 1 calc R . . C19 C 0.2535(10) 1.0517(12) 0.3844(8) 0.089(6) Uani 1 1 d . . . H19 H 0.2203 1.1043 0.3705 0.106 Uiso 1 1 calc R . . N20 N 0.2374(6) 0.9424(9) 0.3862(6) 0.072(4) Uani 1 1 d . . . H20 H 0.1966 0.9217 0.3756 0.087 Uiso 1 1 calc R . . C21 C 0.1776(9) 0.6611(12) 0.5586(7) 0.101(6) Uani 1 1 d . . . H21A H 0.1493 0.6033 0.5376 0.152 Uiso 1 1 calc R . . H21B H 0.1556 0.6966 0.5891 0.152 Uiso 1 1 calc R . . H21C H 0.2186 0.6275 0.5783 0.152 Uiso 1 1 calc R . . C22 C 0.1134(7) 0.8354(12) 0.4691(7) 0.080(5) Uani 1 1 d . . . H22A H 0.1202 0.8919 0.4393 0.120 Uiso 1 1 calc R . . H22B H 0.0943 0.8703 0.5016 0.120 Uiso 1 1 calc R . . H22C H 0.0838 0.7779 0.4496 0.120 Uiso 1 1 calc R . . C23 C 0.2506(8) 0.8797(12) 0.5443(7) 0.090(5) Uani 1 1 d . . . H23A H 0.2603 0.9366 0.5157 0.136 Uiso 1 1 calc R . . H23B H 0.2913 0.8452 0.5639 0.136 Uiso 1 1 calc R . . H23C H 0.2284 0.9144 0.5749 0.136 Uiso 1 1 calc R . . C24 C 0.2889(9) 0.6054(13) 0.2356(7) 0.096(5) Uani 1 1 d . . . H24A H 0.2980 0.5297 0.2510 0.143 Uiso 1 1 calc R . . H24B H 0.3111 0.6177 0.2008 0.143 Uiso 1 1 calc R . . H24C H 0.2418 0.6149 0.2232 0.143 Uiso 1 1 calc R . . C25 C 0.4102(7) 0.6854(14) 0.3174(8) 0.099(6) Uani 1 1 d . . . H25A H 0.4272 0.7380 0.3496 0.148 Uiso 1 1 calc R . . H25B H 0.4317 0.6984 0.2822 0.148 Uiso 1 1 calc R . . H25C H 0.4190 0.6091 0.3320 0.148 Uiso 1 1 calc R . . C26 C 0.3019(8) 0.8504(12) 0.2640(7) 0.090(5) Uani 1 1 d . . . H26A H 0.3177 0.9053 0.2952 0.134 Uiso 1 1 calc R . . H26B H 0.2548 0.8599 0.2511 0.134 Uiso 1 1 calc R . . H26C H 0.3244 0.8612 0.2292 0.134 Uiso 1 1 calc R . . C27 C -0.0039(7) 0.5003(19) 0.1530(8) 0.127(5) Uani 1 1 d D . . H27A H -0.0098 0.5796 0.1413 0.152 Uiso 1 1 calc R . . H27B H -0.0113 0.4572 0.1148 0.152 Uiso 1 1 calc R . . C28 C -0.0575(9) 0.473(2) 0.1845(7) 0.127(5) Uani 1 1 d D . . H28A H -0.0736 0.3974 0.1717 0.152 Uiso 1 1 calc R . . H28B H -0.0937 0.5256 0.1718 0.152 Uiso 1 1 calc R . . C29 C 0.0860(13) 0.3884(19) 0.1543(10) 0.163(5) Uani 1 1 d D . . H29A H 0.1324 0.3781 0.1703 0.245 Uiso 1 1 calc R . . H29B H 0.0799 0.3929 0.1101 0.245 Uiso 1 1 calc R . . H29C H 0.0611 0.3253 0.1663 0.245 Uiso 1 1 calc R . . C30 C 0.0955(13) 0.5834(19) 0.1575(10) 0.163(5) Uani 1 1 d D . . H30A H 0.0781 0.6508 0.1738 0.245 Uiso 1 1 calc R . . H30B H 0.0872 0.5864 0.1132 0.245 Uiso 1 1 calc R . . H30C H 0.1426 0.5787 0.1718 0.245 Uiso 1 1 calc R . . C31 C -0.0750(12) 0.3790(18) 0.2712(10) 0.163(5) Uani 1 1 d D . . H31A H -0.0590 0.3104 0.2551 0.245 Uiso 1 1 calc R . . H31B H -0.1222 0.3854 0.2577 0.245 Uiso 1 1 calc R . . H31C H -0.0659 0.3770 0.3155 0.245 Uiso 1 1 calc R . . C32 C -0.0681(13) 0.5741(18) 0.2730(10) 0.163(5) Uani 1 1 d D . . H32A H -0.0462 0.6395 0.2596 0.245 Uiso 1 1 calc R . . H32B H -0.0607 0.5714 0.3173 0.245 Uiso 1 1 calc R . . H32C H -0.1151 0.5789 0.2580 0.245 Uiso 1 1 calc R . . C33 C 0.4302(16) 0.181(3) 0.2782(18) 0.263(18) Uiso 1 1 d . . . H33A H 0.4126 0.1391 0.2418 0.395 Uiso 1 1 calc R . . H33B H 0.4521 0.2485 0.2668 0.395 Uiso 1 1 calc R . . H33C H 0.3945 0.2027 0.2996 0.395 Uiso 1 1 calc R . . C34 C 0.4951(13) 0.013(2) 0.3061(13) 0.146(9) Uiso 1 1 d . . . H34 H 0.4786 -0.0218 0.2687 0.175 Uiso 1 1 calc R . . C35 C 0.5362(16) -0.040(3) 0.3465(17) 0.194(12) Uiso 1 1 d . . . H35 H 0.5498 -0.1131 0.3393 0.233 Uiso 1 1 calc R . . C36 C 0.5600(15) 0.015(2) 0.4009(16) 0.182(12) Uiso 1 1 d . . . H36 H 0.5877 -0.0242 0.4316 0.219 Uiso 1 1 calc R . . C37 C 0.5448(13) 0.123(2) 0.4114(14) 0.160(9) Uiso 1 1 d . . . H37 H 0.5653 0.1569 0.4479 0.192 Uiso 1 1 calc R . . C38 C 0.4982(12) 0.190(2) 0.3693(12) 0.154(9) Uiso 1 1 d . . . H38 H 0.4849 0.2649 0.3740 0.184 Uiso 1 1 calc R . . C39 C 0.4767(12) 0.113(2) 0.3174(12) 0.135(8) Uiso 1 1 d . . . 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 0.0581(3) 0.0364(2) 0.0369(2) 0.0005(2) 0.00557(16) -0.0034(2) Cl1 0.087(3) 0.0606(19) 0.082(3) -0.0097(17) 0.025(2) 0.0125(18) Cl2 0.084(3) 0.0518(17) 0.078(2) -0.0100(16) -0.024(2) 0.0078(17) Cl3 0.094(3) 0.0506(17) 0.066(2) -0.0122(15) -0.009(2) -0.0022(17) Si1 0.058(3) 0.0579(19) 0.052(2) 0.0070(16) 0.0109(18) -0.0040(17) Si2 0.053(3) 0.111(3) 0.067(3) 0.025(2) -0.006(2) -0.014(2) Si3 0.070(3) 0.0464(17) 0.0407(19) -0.0056(14) 0.0093(17) -0.0055(16) Si4 0.088(3) 0.055(2) 0.049(2) -0.0014(16) 0.022(2) -0.0098(19) N1 0.038(6) 0.044(5) 0.039(5) 0.009(4) 0.009(5) -0.004(4) N2 0.034(6) 0.073(6) 0.034(5) 0.007(4) 0.000(4) -0.006(5) N3 0.046(6) 0.037(4) 0.046(6) -0.010(4) 0.009(5) -0.008(4) N4 0.057(7) 0.042(5) 0.048(6) 0.000(4) 0.018(5) -0.009(5) N5 0.083(9) 0.061(7) 0.054(6) -0.007(5) 0.012(6) 0.005(6) N6 0.068(8) 0.070(7) 0.048(6) -0.005(5) -0.005(5) -0.009(6) Li1 0.076(18) 0.113(19) 0.036(11) -0.017(12) 0.010(11) 0.011(14) C1 0.057(9) 0.029(5) 0.070(9) -0.005(5) 0.005(7) 0.002(5) C2 0.057(9) 0.058(7) 0.035(6) 0.004(5) -0.001(6) -0.003(6) N31 0.116(12) 0.063(7) 0.074(9) 0.010(6) 0.022(8) 0.011(7) C4 0.112(14) 0.092(11) 0.039(8) 0.003(7) 0.015(8) 0.008(9) C5 0.085(13) 0.078(10) 0.068(11) 0.023(8) -0.002(9) -0.018(8) C6 0.079(12) 0.066(8) 0.070(10) 0.021(8) -0.008(8) 0.001(8) C7 0.065(9) 0.044(6) 0.046(7) -0.001(5) 0.003(6) -0.001(6) C8 0.052(11) 0.192(19) 0.119(15) 0.107(14) -0.001(10) -0.004(11) C9 0.082(13) 0.106(12) 0.090(12) -0.006(10) 0.032(10) -0.026(10) C10 0.092(14) 0.068(9) 0.095(12) -0.014(8) 0.022(10) -0.023(8) C11 0.057(10) 0.082(10) 0.113(13) 0.039(9) 0.000(9) -0.018(8) C12 0.055(13) 0.142(18) 0.34(4) 0.14(2) -0.005(18) 0.009(12) C13 0.117(19) 0.50(5) 0.082(14) -0.01(2) 0.013(13) -0.18(3) C14 0.045(8) 0.047(6) 0.056(8) -0.012(6) 0.007(6) -0.009(5) C15 0.054(9) 0.038(6) 0.051(7) 0.000(5) 0.013(6) -0.004(6) C16 0.078(12) 0.061(8) 0.068(9) 0.003(7) 0.009(8) -0.008(8) C17 0.098(13) 0.076(11) 0.103(13) -0.011(10) 0.007(10) -0.061(11) C18 0.17(2) 0.038(7) 0.081(12) 0.003(8) 0.036(13) -0.013(10) C19 0.144(18) 0.040(7) 0.087(12) 0.003(8) 0.033(12) 0.010(9) N20 0.077(10) 0.047(6) 0.095(10) 0.010(6) 0.022(8) -0.009(6) C21 0.169(19) 0.068(9) 0.085(12) 0.010(8) 0.074(12) 0.024(10) C22 0.084(13) 0.092(10) 0.066(10) -0.018(8) 0.016(9) 0.026(9) C23 0.125(15) 0.081(10) 0.060(9) -0.031(8) 0.000(9) -0.024(9) C24 0.138(17) 0.095(12) 0.056(9) -0.006(8) 0.022(10) -0.015(11) C25 0.075(13) 0.118(13) 0.113(14) -0.024(11) 0.045(11) -0.014(10) C26 0.118(15) 0.083(10) 0.073(11) 0.024(8) 0.031(10) -0.001(9) C27 0.081(10) 0.215(16) 0.076(9) 0.012(11) -0.013(7) -0.016(12) C28 0.081(10) 0.215(16) 0.076(9) 0.012(11) -0.013(7) -0.016(12) C29 0.216(15) 0.174(11) 0.099(8) 0.003(9) 0.021(9) -0.002(11) C30 0.216(15) 0.174(11) 0.099(8) 0.003(9) 0.021(9) -0.002(11) C31 0.216(15) 0.174(11) 0.099(8) 0.003(9) 0.021(9) -0.002(11) C32 0.216(15) 0.174(11) 0.099(8) 0.003(9) 0.021(9) -0.002(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 N2 2.458(9) . ? Th1 N4 2.464(8) . ? Th1 N1 2.503(8) . ? Th1 N3 2.508(8) . ? Th1 Cl1 2.686(4) . ? Th1 Cl2 2.815(3) . ? Th1 Cl3 2.814(3) . ? Th1 C1 2.843(13) . ? Th1 C14 2.880(11) . ? Cl2 Li1 2.38(2) . ? Cl3 Li1 2.41(3) . ? Si1 N1 1.736(9) . ? Si1 C8 1.834(15) . ? Si1 C9 1.809(16) . ? Si1 C10 1.839(13) . ? Si2 N2 1.737(10) . ? Si2 C12 1.841(19) . ? Si2 C11 1.829(14) . ? Si2 C13 1.82(2) . ? Si3 N3 1.751(9) . ? Si3 C21 1.854(14) . ? Si3 C23 1.861(13) . ? Si3 C22 1.877(14) . ? Si4 N4 1.745(10) . ? Si4 C24 1.797(15) . ? Si4 C26 1.844(14) . ? Si4 C25 1.859(16) . ? N1 C1 1.323(14) . ? N2 C1 1.320(14) . ? N3 C14 1.321(14) . ? N4 C14 1.350(14) . ? N5 C29 1.38(2) . ? N5 C27 1.405(15) . ? N5 C30 1.41(2) . ? N5 Li1 2.03(2) . ? N6 C32 1.417(19) . ? N6 C31 1.427(19) . ? N6 C28 1.414(15) . ? N6 Li1 2.12(3) . ? Li1 C27 2.73(3) . ? C1 C2 1.531(16) . ? C2 N31 1.346(15) . ? C2 C7 1.341(15) . ? N31 C4 1.329(17) . ? N31 H31 0.8600 . ? C4 C5 1.361(19) . ? C4 H4 0.9300 . ? C5 C6 1.31(2) . ? C5 H5 0.9300 . ? C6 C7 1.387(18) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.512(14) . ? C15 N20 1.304(15) . ? C15 C16 1.342(17) . ? C16 C17 1.419(17) . ? C16 H16 0.9300 . ? C17 C18 1.32(2) . ? C17 H17 0.9300 . ? C18 C19 1.41(2) . ? C18 H18 0.9300 . ? C19 N20 1.330(18) . ? C19 H19 0.9300 . ? N20 H20 0.8600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.422(16) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C39 1.42(3) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.27(3) . ? C34 C39 1.28(3) . ? C34 H34 0.9300 . ? C35 C36 1.38(4) . ? C35 H35 0.9300 . ? C36 C37 1.33(3) . ? C36 H36 0.9300 . ? C37 C38 1.45(3) . ? C37 H37 0.9300 . ? C38 C39 1.47(3) . ? C38 H38 0.9300 . ? 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 N2 Th1 N4 106.9(3) . . ? N2 Th1 N1 55.3(3) . . ? N4 Th1 N1 151.7(3) . . ? N2 Th1 N3 81.4(3) . . ? N4 Th1 N3 55.2(3) . . ? N1 Th1 N3 97.9(3) . . ? N2 Th1 Cl1 80.9(2) . . ? N4 Th1 Cl1 83.1(2) . . ? N1 Th1 Cl1 111.9(2) . . ? N3 Th1 Cl1 126.5(2) . . ? N2 Th1 Cl2 142.3(2) . . ? N4 Th1 Cl2 82.8(2) . . ? N1 Th1 Cl2 99.3(2) . . ? N3 Th1 Cl2 74.7(2) . . ? Cl1 Th1 Cl2 136.82(12) . . ? N2 Th1 Cl3 122.7(2) . . ? N4 Th1 Cl3 123.5(2) . . ? N1 Th1 Cl3 83.8(2) . . ? N3 Th1 Cl3 149.0(2) . . ? Cl1 Th1 Cl3 79.92(12) . . ? Cl2 Th1 Cl3 74.51(10) . . ? N2 Th1 C1 27.6(3) . . ? N4 Th1 C1 132.2(3) . . ? N1 Th1 C1 27.7(3) . . ? N3 Th1 C1 91.2(3) . . ? Cl1 Th1 C1 95.5(3) . . ? Cl2 Th1 C1 123.6(3) . . ? Cl3 Th1 C1 102.9(2) . . ? N2 Th1 C14 95.2(3) . . ? N4 Th1 C14 27.9(3) . . ? N1 Th1 C14 124.9(3) . . ? N3 Th1 C14 27.3(3) . . ? Cl1 Th1 C14 106.3(3) . . ? Cl2 Th1 C14 76.4(3) . . ? Cl3 Th1 C14 142.0(3) . . ? C1 Th1 C14 113.4(3) . . ? Li1 Cl2 Th1 97.6(6) . . ? Li1 Cl3 Th1 96.9(6) . . ? N1 Si1 C8 107.8(6) . . ? N1 Si1 C9 112.0(6) . . ? C8 Si1 C9 108.5(8) . . ? N1 Si1 C10 111.8(6) . . ? C8 Si1 C10 106.4(9) . . ? C9 Si1 C10 110.1(7) . . ? N2 Si2 C12 112.2(8) . . ? N2 Si2 C11 105.3(6) . . ? C12 Si2 C11 109.4(9) . . ? N2 Si2 C13 113.2(8) . . ? C12 Si2 C13 110.3(13) . . ? C11 Si2 C13 106.1(10) . . ? N3 Si3 C21 108.3(5) . . ? N3 Si3 C23 114.6(6) . . ? C21 Si3 C23 108.3(8) . . ? N3 Si3 C22 109.8(6) . . ? C21 Si3 C22 106.5(8) . . ? C23 Si3 C22 109.1(7) . . ? N4 Si4 C24 106.8(6) . . ? N4 Si4 C26 113.9(6) . . ? C24 Si4 C26 108.4(8) . . ? N4 Si4 C25 109.8(7) . . ? C24 Si4 C25 108.1(8) . . ? C26 Si4 C25 109.6(8) . . ? C1 N1 Si1 129.5(8) . . ? C1 N1 Th1 90.6(7) . . ? Si1 N1 Th1 139.2(5) . . ? C1 N2 Si2 130.5(9) . . ? C1 N2 Th1 92.6(7) . . ? Si2 N2 Th1 136.5(5) . . ? C14 N3 Si3 129.1(7) . . ? C14 N3 Th1 92.2(6) . . ? Si3 N3 Th1 138.1(5) . . ? C14 N4 Si4 130.2(8) . . ? C14 N4 Th1 93.4(7) . . ? Si4 N4 Th1 136.0(5) . . ? C29 N5 C27 108.1(16) . . ? C29 N5 C30 111.7(18) . . ? C27 N5 C30 105.1(15) . . ? C29 N5 Li1 110.5(14) . . ? C27 N5 Li1 103.4(12) . . ? C30 N5 Li1 117.3(14) . . ? C32 N6 C31 108.0(17) . . ? C32 N6 C28 110.2(16) . . ? C31 N6 C28 106.6(14) . . ? C32 N6 Li1 111.1(14) . . ? C31 N6 Li1 115.7(14) . . ? C28 N6 Li1 105.1(11) . . ? N5 Li1 N6 87.6(10) . . ? N5 Li1 Cl2 120.2(13) . . ? N6 Li1 Cl2 112.7(10) . . ? N5 Li1 Cl3 109.7(10) . . ? N6 Li1 Cl3 139.3(13) . . ? Cl2 Li1 Cl3 90.6(8) . . ? N5 Li1 C27 30.1(5) . . ? N6 Li1 C27 57.6(7) . . ? Cl2 Li1 C27 125.8(12) . . ? Cl3 Li1 C27 133.5(10) . . ? N1 C1 N2 121.1(11) . . ? N1 C1 C2 120.1(11) . . ? N2 C1 C2 118.9(11) . . ? N1 C1 Th1 61.7(6) . . ? N2 C1 Th1 59.7(6) . . ? C2 C1 Th1 174.8(8) . . ? N31 C2 C7 120.8(11) . . ? N31 C2 C1 116.9(10) . . ? C7 C2 C1 122.2(11) . . ? C4 N31 C2 118.0(12) . . ? C4 N31 H31 121.0 . . ? C2 N31 H31 121.0 . . ? N31 C4 C5 122.9(14) . . ? N31 C4 H4 118.5 . . ? C5 C4 H4 118.5 . . ? C6 C5 C4 118.9(14) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? C5 C6 C7 119.8(13) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C2 C7 C6 119.6(13) . . ? C2 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 N4 119.1(9) . . ? N3 C14 C15 121.6(10) . . ? N4 C14 C15 119.1(11) . . ? N3 C14 Th1 60.5(5) . . ? N4 C14 Th1 58.6(5) . . ? C15 C14 Th1 177.6(9) . . ? N20 C15 C16 122.5(11) . . ? N20 C15 C14 116.9(11) . . ? C16 C15 C14 120.5(11) . . ? C15 C16 C17 117.0(14) . . ? C15 C16 H16 121.5 . . ? C17 C16 H16 121.5 . . ? C18 C17 C16 122.2(16) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C17 C18 C19 115.9(14) . . ? C17 C18 H18 122.1 . . ? C19 C18 H18 122.1 . . ? N20 C19 C18 121.9(16) . . ? N20 C19 H19 119.0 . . ? C18 C19 H19 119.0 . . ? C15 N20 C19 120.3(14) . . ? C15 N20 H20 119.8 . . ? C19 N20 H20 119.8 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si4 C24 H24A 109.5 . . ? Si4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si4 C25 H25A 109.5 . . ? Si4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 N5 124.7(16) . . ? C28 C27 Li1 79.7(11) . . ? N5 C27 Li1 46.5(9) . . ? C28 C27 H27A 106.2 . . ? N5 C27 H27A 106.2 . . ? Li1 C27 H27A 112.8 . . ? C28 C27 H27B 106.2 . . ? N5 C27 H27B 106.2 . . ? Li1 C27 H27B 137.0 . . ? H27A C27 H27B 106.4 . . ? C27 C28 N6 115.4(14) . . ? C27 C28 H28A 108.4 . . ? N6 C28 H28A 108.4 . . ? C27 C28 H28B 108.4 . . ? N6 C28 H28B 108.4 . . ? H28A C28 H28B 107.5 . . ? N5 C29 H29A 109.4 . . ? N5 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N5 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N5 C30 H30A 109.5 . . ? N5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N6 C31 H31A 109.5 . . ? N6 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N6 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N6 C32 H32A 109.5 . . ? N6 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N6 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C39 C33 H33A 109.5 . . ? C39 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C39 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C39 119(3) . . ? C35 C34 H34 120.3 . . ? C39 C34 H34 120.3 . . ? C34 C35 C36 118(3) . . ? C34 C35 H35 120.8 . . ? C36 C35 H35 120.8 . . ? C37 C36 C35 123(3) . . ? C37 C36 H36 118.7 . . ? C35 C36 H36 118.7 . . ? C36 C37 C38 124(3) . . ? C36 C37 H37 118.1 . . ? C38 C37 H37 118.1 . . ? C39 C38 C37 104(2) . . ? C39 C38 H38 128.1 . . ? C37 C38 H38 128.1 . . ? C34 C39 C33 126(3) . . ? C34 C39 C38 132(3) . . ? C33 C39 C38 102(2) . . ? loop_ # start Validation Reply Form _vrf_PLAT220_complex2 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ...4.96 Ratio RESPONSE: Unresolved disorder at TMDA-molecule ; _vrf_PLAT222_complex2 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ...5.54 Ratio RESPONSE: Unresolved disorder at TMDA-molecule ; _vrf_PLAT242_complex2 ; PROBLEM: Check Low Ueq as Compared to Neighbors for Si2 RESPONSE: Si2 is connected to disordered Methyl-groups ; # end Validation Reply Form _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.32 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 2.033 _refine_diff_density_min -1.710 _refine_diff_density_rms 0.151 #end data_complex3 _database_code_depnum_ccdc_archive 'CCDC 761285' #TrackingRef 'Th amidinates.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common complex3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H66 Cl N9 Si6 Th' _chemical_formula_weight 1061.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Th Th -7.2400 8.8979 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 15.407(3) _cell_length_b 15.407(3) _cell_length_c 21.160(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4349.9(15) _cell_formula_units_Z 3 _cell_measurement_temperature 240(1) _cell_measurement_reflns_used 11733 _cell_measurement_theta_min 1.80 _cell_measurement_theta_max 25.34 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 2.770 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.492 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details ; 'PLATON (Spek, A.L. 1995)' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11726 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.34 _reflns_number_total 3455 _reflns_number_gt 3427 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2006)' _computing_cell_refinement 'DENZO HKL2000 (Otwinowski & Minor 1997)' _computing_data_reduction 'DENZO HKL2000 (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'TEXSAN (MSC, 1999)' _computing_publication_material ? _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^)+(0.0531P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.097(11) _refine_ls_number_reflns 3455 _refine_ls_number_parameters 148 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Th1 Th 0.6667 0.3333 0.0431 0.02021(13) Uani 1 3 d S . . Cl1 Cl 0.6667 0.3333 -0.08534(15) 0.0349(7) Uani 1 3 d S . . Si1 Si 0.63351(17) 0.08541(16) -0.02399(11) 0.0355(5) Uani 1 1 d . . . Si2 Si 0.4408(3) 0.1780(2) 0.16671(15) 0.0551(8) Uani 1 1 d D . . N1 N 0.5999(4) 0.1532(4) 0.0270(3) 0.0270(13) Uani 1 1 d . . . N2 N 0.5258(5) 0.1932(5) 0.1066(3) 0.0345(15) Uani 1 1 d . . . N3 N 0.3782(7) -0.0270(7) 0.0251(5) 0.069(3) Uani 1 1 d . . . C1 C 0.5266(5) 0.1239(5) 0.0701(4) 0.0297(16) Uani 1 1 d . . . C2 C 0.4494(6) 0.0156(6) 0.0736(4) 0.0346(18) Uani 1 1 d . . . C3 C 0.4540(5) -0.0351(5) 0.1234(3) 0.0270(15) Uani 1 1 d . . . H3 H 0.5014 -0.0036 0.1551 0.032 Uiso 1 1 calc R . . C4 C 0.3872(8) -0.1337(7) 0.1256(5) 0.055(3) Uani 1 1 d . . . H4 H 0.3902 -0.1707 0.1594 0.066 Uiso 1 1 calc R . . C5 C 0.3162(9) -0.1817(7) 0.0815(6) 0.065(3) Uani 1 1 d . . . H5 H 0.2715 -0.2501 0.0849 0.078 Uiso 1 1 calc R . . C6 C 0.3105(8) -0.1281(8) 0.0309(6) 0.066(3) Uani 1 1 d . . . H6 H 0.2608 -0.1604 0.0006 0.079 Uiso 1 1 calc R . . C7 C 0.7710(7) 0.1685(8) -0.0359(5) 0.051(2) Uani 1 1 d . . . H7A H 0.7838 0.2314 -0.0532 0.077 Uiso 1 1 calc R . . H7B H 0.7952 0.1371 -0.0646 0.077 Uiso 1 1 calc R . . H7C H 0.8049 0.1798 0.0039 0.077 Uiso 1 1 calc R . . C8 C 0.6109(8) -0.0358(7) 0.0091(5) 0.054(2) Uani 1 1 d . . . H8A H 0.5403 -0.0794 0.0154 0.081 Uiso 1 1 calc R . . H8B H 0.6452 -0.0242 0.0488 0.081 Uiso 1 1 calc R . . H8C H 0.6356 -0.0665 -0.0198 0.081 Uiso 1 1 calc R . . C9 C 0.5671(10) 0.0605(9) -0.1017(5) 0.058(3) Uani 1 1 d . . . H9A H 0.4964 0.0174 -0.0954 0.087 Uiso 1 1 calc R . . H9B H 0.5916 0.0287 -0.1298 0.087 Uiso 1 1 calc R . . H9C H 0.5791 0.1227 -0.1199 0.087 Uiso 1 1 calc R . . C10 C 0.3167(10) 0.0665(11) 0.1609(8) 0.114(3) Uani 1 1 d D . . H10A H 0.3231 0.0077 0.1614 0.171 Uiso 1 1 calc R . . H10B H 0.2853 0.0687 0.1222 0.171 Uiso 1 1 calc R . . H10C H 0.2764 0.0646 0.1961 0.171 Uiso 1 1 calc R . . C11 C 0.4908(12) 0.1726(13) 0.2450(6) 0.114(3) Uani 1 1 d D . . H11A H 0.5013 0.1163 0.2465 0.171 Uiso 1 1 calc R . . H11B H 0.4437 0.1655 0.2772 0.171 Uiso 1 1 calc R . . H11C H 0.5532 0.2332 0.2521 0.171 Uiso 1 1 calc R . . C12 C 0.4189(13) 0.2847(11) 0.1651(8) 0.114(3) Uani 1 1 d D . . H12A H 0.3943 0.2890 0.1242 0.171 Uiso 1 1 calc R . . H12B H 0.4807 0.3455 0.1735 0.171 Uiso 1 1 calc R . . H12C H 0.3704 0.2756 0.1968 0.171 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 0.01833(14) 0.01833(14) 0.02398(19) 0.000 0.000 0.00917(7) Cl1 0.0375(11) 0.0375(11) 0.0297(16) 0.000 0.000 0.0188(5) Si1 0.0430(12) 0.0312(11) 0.0387(12) -0.0033(9) 0.0029(10) 0.0232(10) Si2 0.068(2) 0.0458(16) 0.0592(19) 0.0181(14) 0.0388(16) 0.0339(15) N1 0.027(3) 0.018(3) 0.036(3) 0.005(3) 0.003(3) 0.011(2) N2 0.037(4) 0.025(3) 0.040(4) 0.001(3) 0.013(3) 0.014(3) N3 0.050(5) 0.052(5) 0.092(7) -0.004(5) -0.015(5) 0.016(4) C1 0.027(4) 0.027(4) 0.035(4) 0.005(3) 0.000(3) 0.013(3) C2 0.030(4) 0.027(4) 0.049(5) -0.003(4) 0.002(4) 0.016(3) C3 0.029(4) 0.021(4) 0.025(4) 0.005(3) 0.001(3) 0.008(3) C4 0.064(6) 0.045(5) 0.054(6) 0.018(5) 0.023(5) 0.025(5) C5 0.066(7) 0.029(5) 0.076(7) 0.006(5) 0.010(6) 0.005(5) C6 0.049(6) 0.041(5) 0.080(8) -0.005(5) -0.013(6) 0.002(5) C7 0.050(5) 0.059(6) 0.053(6) 0.001(5) 0.016(4) 0.034(5) C8 0.073(7) 0.039(5) 0.063(6) 0.004(4) 0.016(5) 0.038(5) C9 0.086(8) 0.051(6) 0.035(5) -0.001(5) -0.010(5) 0.033(6) C10 0.132(8) 0.120(7) 0.116(7) 0.026(6) 0.068(6) 0.082(7) C11 0.132(8) 0.120(7) 0.116(7) 0.026(6) 0.068(6) 0.082(7) C12 0.132(8) 0.120(7) 0.116(7) 0.026(6) 0.068(6) 0.082(7) _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 2.454(6) . ? Th1 N1 2.454(6) 2_655 ? Th1 N1 2.454(6) 3_665 ? Th1 N2 2.548(6) 2_655 ? Th1 N2 2.548(6) . ? Th1 N2 2.548(6) 3_665 ? Th1 Cl1 2.718(3) . ? Th1 C1 2.903(7) 2_655 ? Th1 C1 2.903(7) . ? Th1 C1 2.903(7) 3_665 ? Si1 N1 1.750(6) . ? Si1 C8 1.857(9) . ? Si1 C7 1.865(9) . ? Si1 C9 1.873(11) . ? Si2 N2 1.755(7) . ? Si2 C10 1.827(13) . ? Si2 C12 1.836(12) . ? Si2 C11 1.846(14) . ? N1 C1 1.342(10) . ? N2 C1 1.322(10) . ? N3 C6 1.380(13) . ? N3 C2 1.402(13) . ? C1 C2 1.490(10) . ? C2 C3 1.335(11) . ? C3 C4 1.344(12) . ? C3 H3 0.9300 . ? C4 C5 1.344(16) . ? C4 H4 0.9300 . ? C5 C6 1.380(16) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? 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 N1 118.10(7) . 2_655 ? N1 Th1 N1 118.10(7) . 3_665 ? N1 Th1 N1 118.10(7) 2_655 3_665 ? N1 Th1 N2 86.9(2) . 2_655 ? N1 Th1 N2 54.4(2) 2_655 2_655 ? N1 Th1 N2 149.0(2) 3_665 2_655 ? N1 Th1 N2 54.4(2) . . ? N1 Th1 N2 149.0(2) 2_655 . ? N1 Th1 N2 86.9(2) 3_665 . ? N2 Th1 N2 94.7(2) 2_655 . ? N1 Th1 N2 149.0(2) . 3_665 ? N1 Th1 N2 86.9(2) 2_655 3_665 ? N1 Th1 N2 54.4(2) 3_665 3_665 ? N2 Th1 N2 94.7(2) 2_655 3_665 ? N2 Th1 N2 94.7(2) . 3_665 ? N1 Th1 Cl1 82.00(14) . . ? N1 Th1 Cl1 82.00(14) 2_655 . ? N1 Th1 Cl1 82.00(14) 3_665 . ? N2 Th1 Cl1 121.83(15) 2_655 . ? N2 Th1 Cl1 121.83(15) . . ? N2 Th1 Cl1 121.83(15) 3_665 . ? N1 Th1 C1 101.8(2) . 2_655 ? N1 Th1 C1 27.4(2) 2_655 2_655 ? N1 Th1 C1 140.0(2) 3_665 2_655 ? N2 Th1 C1 27.1(2) 2_655 2_655 ? N2 Th1 C1 121.8(2) . 2_655 ? N2 Th1 C1 93.0(2) 3_665 2_655 ? Cl1 Th1 C1 101.35(15) . 2_655 ? N1 Th1 C1 27.4(2) . . ? N1 Th1 C1 140.0(2) 2_655 . ? N1 Th1 C1 101.8(2) 3_665 . ? N2 Th1 C1 93.0(2) 2_655 . ? N2 Th1 C1 27.1(2) . . ? N2 Th1 C1 121.8(2) 3_665 . ? Cl1 Th1 C1 101.35(15) . . ? C1 Th1 C1 116.23(10) 2_655 . ? N1 Th1 C1 140.0(2) . 3_665 ? N1 Th1 C1 101.8(2) 2_655 3_665 ? N1 Th1 C1 27.4(2) 3_665 3_665 ? N2 Th1 C1 121.8(2) 2_655 3_665 ? N2 Th1 C1 93.0(2) . 3_665 ? N2 Th1 C1 27.1(2) 3_665 3_665 ? Cl1 Th1 C1 101.35(15) . 3_665 ? C1 Th1 C1 116.22(10) 2_655 3_665 ? C1 Th1 C1 116.22(10) . 3_665 ? N1 Si1 C8 113.9(4) . . ? N1 Si1 C7 104.3(4) . . ? C8 Si1 C7 108.6(5) . . ? N1 Si1 C9 111.6(4) . . ? C8 Si1 C9 108.5(5) . . ? C7 Si1 C9 109.8(5) . . ? N2 Si2 C10 115.9(5) . . ? N2 Si2 C12 109.0(5) . . ? C10 Si2 C12 105.5(8) . . ? N2 Si2 C11 110.8(5) . . ? C10 Si2 C11 106.4(8) . . ? C12 Si2 C11 108.9(8) . . ? C1 N1 Si1 132.0(5) . . ? C1 N1 Th1 95.3(4) . . ? Si1 N1 Th1 132.8(3) . . ? C1 N2 Si2 128.6(5) . . ? C1 N2 Th1 91.6(4) . . ? Si2 N2 Th1 139.3(3) . . ? C6 N3 C2 115.9(9) . . ? N2 C1 N1 118.2(6) . . ? N2 C1 C2 123.4(7) . . ? N1 C1 C2 118.4(7) . . ? N2 C1 Th1 61.3(4) . . ? N1 C1 Th1 57.3(4) . . ? C2 C1 Th1 171.0(6) . . ? C3 C2 N3 124.2(8) . . ? C3 C2 C1 116.6(7) . . ? N3 C2 C1 119.2(8) . . ? C2 C3 C4 117.0(8) . . ? C2 C3 H3 121.5 . . ? C4 C3 H3 121.5 . . ? C3 C4 C5 123.3(9) . . ? C3 C4 H4 118.3 . . ? C5 C4 H4 118.3 . . ? C4 C5 C6 119.2(9) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C5 C6 N3 120.4(10) . . ? C5 C6 H6 119.8 . . ? N3 C6 H6 119.8 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? # start Validation Reply Form _vrf_PLAT222_complex3 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.34 Ratio RESPONSE: Slightly disordered methyl groups. ; _vrf_PLAT601_complex3 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 335.00 A**3 RESPONSE: No solvent molecules were founded at the crystal structure. ; # end Validation Reply Form_diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.001 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.144