# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2285 data_global _publ_contact_letter ; These are the CIF format data (3 compounds) for the paper "New main group and early transition metal complexes of mono-pendant arm triazacyclononane ligands " S. Y. Bylikin, N. A. H. Male, D. A. Robson, L. H. Rees, P. Mountford and M. Schroeder ; _publ_contact_author ; Dr P. Mountford Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; _publ_contact_author_phone '+44 1865 272679' _contact_author_fax '+44 1865 272690' _publ_contact_author_email Philip.Mountford@chem.ox.ac.uk data_Compound_5b # local code str57 _chemical_name_systematic ; [In(L-b)Cl2] ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _cell_length_a 10.285(8) _cell_angle_alpha 90 _cell_length_b 14.613(6) _cell_angle_beta 99.539(6) _cell_length_c 26.906(4) _cell_angle_gamma 90 _cell_volume 3987.9(5) _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' 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 '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 57.7997 0.0030 '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' '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' 'In ' -0.9360 1.3100 19.1624 0.5476 18.5596 6.3776 4.2948 25.8499 2.0396 92.8029 4.9391 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum 'C30 H54 Cl8 In N3 O' _chemical_formula_moiety 'C27 H48 Cl2 In N3 O, 3(C H2 Cl2)' _chemical_compound_source ; K[L-b] + InCl3 ; _chemical_formula_weight 871.23 _cell_measurement_reflns_used 35607 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.45 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1792.65 _exptl_absorpt_coefficient_mu 1.16 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'refined from delta-F (Walker & Stuart , 1983)' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.84 _diffrn_measurement_device_type ; Enraf-nonius DIP2000 ; _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 35607 _reflns_number_total 7300 _diffrn_reflns_av_R_equivalents 0.06 _diffrn_measured_fraction_theta_max 0.876 _reflns_number_gt 3480 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 33 _refine_diff_density_min -0.98 _refine_diff_density_max 0.85 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 3480 _refine_ls_number_parameters 388 _refine_ls_R_factor_gt 0.0958 _refine_ls_wR_factor_ref 0.0178 _refine_ls_goodness_of_fit_ref 0.9379 _refine_ls_shift/su_max 0.0003 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 2.34 -5.21 0.712 ; _refine_ls_extinction_coef 'none required' _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _computing_data_collection ; DIP2000 software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' loop_ _atom_site_label _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 In1 0.91390(6) 0.23824(4) 0.21216(2) 0.0221 1.0000 Uani Cl1 1.0998(2) 0.34408(16) 0.2236(1) 0.0338 1.0000 Uani Cl2 0.7505(2) 0.3510(2) 0.23369(9) 0.0410 1.0000 Uani Cl3 0.4893(5) 0.5284(3) 0.1338(2) 0.1334 1.0000 Uani Cl4 0.3482(3) 0.3628(3) 0.14731(12) 0.0891 1.0000 Uani Cl5 0.4467(3) 0.2211(3) 0.29104(17) 0.0905 1.0000 Uani Cl6 0.4607(4) 0.3970(2) 0.33763(12) 0.0747 1.0000 Uani Cl7 0.9922(4) 0.1205(3) -0.01292(16) 0.0952 1.0000 Uani Cl8 0.7348(4) 0.0822(3) -0.06613(14) 0.0895 1.0000 Uani N1 0.7725(7) 0.1198(5) 0.1910(3) 0.0313 1.0000 Uani N4 0.9102(8) 0.1683(6) 0.2912(3) 0.0442 1.0000 Uani N7 1.0649(8) 0.1138(5) 0.2092(3) 0.0289 1.0000 Uani O18 0.8660(5) 0.2727(5) 0.1365(2) 0.0362 1.0000 Uani C2 0.739(1) 0.0799(9) 0.2355(4) 0.0438 1.0000 Uani C3 0.7723(9) 0.1299(7) 0.2842(4) 0.0365 1.0000 Uani C5 1.0051(9) 0.0934(7) 0.2970(4) 0.0403 1.0000 Uani C6 1.1175(9) 0.1016(7) 0.2642(3) 0.0332 1.0000 Uani C8 0.9816(9) 0.0322(6) 0.1885(4) 0.0347 1.0000 Uani C9 0.8467(9) 0.0567(7) 0.1605(3) 0.0358 1.0000 Uani C11 0.6455(9) 0.1494(7) 0.1589(3) 0.0391 1.0000 Uani C12 0.6532(8) 0.1989(6) 0.1098(3) 0.0310 1.0000 Uani C13 0.5429(9) 0.1872(7) 0.0727(3) 0.0309 1.0000 Uani C14 0.5260(8) 0.2372(9) 0.0285(3) 0.0410 1.0000 Uani C15 0.622(1) 0.3038(7) 0.0224(3) 0.0364 1.0000 Uani C16 0.735(1) 0.3144(7) 0.0584(4) 0.0327 1.0000 Uani C17 0.7511(8) 0.2619(8) 0.1020(3) 0.0320 1.0000 Uani C41 0.9269(8) 0.2353(7) 0.3368(3) 0.0339 1.0000 Uani C42 1.0626(11) 0.2746(7) 0.3479(4) 0.0465 1.0000 Uani C43 0.8853(12) 0.1886(9) 0.3827(3) 0.0594 1.0000 Uani C71 1.1711(9) 0.1327(7) 0.1800(4) 0.0406 1.0000 Uani C72 1.123(1) 0.1452(7) 0.1257(4) 0.0466 1.0000 Uani C73 1.280(1) 0.0560(9) 0.1889(4) 0.0559 1.0000 Uani C81 0.4924(11) 0.4073(8) 0.1286(5) 0.0584 1.0000 Uani C91 0.4446(11) 0.3375(11) 0.2799(4) 0.0662 1.0000 Uani C101 0.8268(14) 0.0980(9) -0.0077(5) 0.0726 1.0000 Uani C141 0.403(1) 0.2236(8) -0.0122(5) 0.0464 1.0000 Uani C142 0.2873(9) 0.2662(12) 0.0070(4) 0.0734 1.0000 Uani C143 0.421(1) 0.2630(14) -0.0624(4) 0.0799 1.0000 Uani C144 0.3796(15) 0.122(1) -0.0231(5) 0.0826 1.0000 Uani C161 0.8347(9) 0.3945(7) 0.0499(3) 0.0353 1.0000 Uani C162 0.8417(12) 0.4629(8) 0.0924(3) 0.0510 1.0000 Uani C163 0.9678(11) 0.3546(8) 0.0490(5) 0.0535 1.0000 Uani C164 0.7865(13) 0.4428(9) 0.0012(4) 0.0586 1.0000 Uani H91 0.8559 0.0868 0.1284 0.0600 1.0000 Uiso H92 0.7938 -0.0009 0.1526 0.0600 1.0000 Uiso H151 0.6088 0.3427 -0.0078 0.0600 1.0000 Uiso H731 1.3518 0.0688 0.1696 0.0600 1.0000 Uiso H732 1.3181 0.0502 0.2254 0.0600 1.0000 Uiso H733 1.2394 -0.0047 0.1775 0.0600 1.0000 Uiso H131 0.4745 0.1423 0.0782 0.0600 1.0000 Uiso H711 1.2140 0.1911 0.1939 0.0600 1.0000 Uiso H421 1.0689 0.3174 0.3764 0.0600 1.0000 Uiso H422 1.1268 0.2242 0.3562 0.0600 1.0000 Uiso H423 1.0827 0.3077 0.3177 0.0600 1.0000 Uiso H81 1.0294 -0.0030 0.1657 0.0600 1.0000 Uiso H82 0.9699 -0.0083 0.2176 0.0600 1.0000 Uiso H31 0.7656 0.0876 0.3125 0.0600 1.0000 Uiso H32 0.7098 0.1813 0.2848 0.0600 1.0000 Uiso H721 1.1972 0.1590 0.1075 0.0600 1.0000 Uiso H722 1.0599 0.1984 0.1205 0.0600 1.0000 Uiso H723 1.0762 0.0901 0.1112 0.0600 1.0000 Uiso H21 0.7850 0.0199 0.2403 0.0600 1.0000 Uiso H22 0.6432 0.0704 0.2295 0.0600 1.0000 Uiso H1421 0.2053 0.2559 -0.0184 0.0600 1.0000 Uiso H1422 0.3025 0.3310 0.0124 0.0600 1.0000 Uiso H1423 0.2750 0.2352 0.0389 0.0600 1.0000 Uiso H811 0.5723 0.3828 0.1509 0.0600 1.0000 Uiso H812 0.4970 0.3897 0.0933 0.0600 1.0000 Uiso H1631 1.0289 0.4060 0.0435 0.0600 1.0000 Uiso H1632 1.0010 0.3248 0.0812 0.0600 1.0000 Uiso H1633 0.9638 0.3110 0.0209 0.0600 1.0000 Uiso H111 0.6003 0.1907 0.1796 0.0600 1.0000 Uiso H112 0.5904 0.0938 0.1502 0.0600 1.0000 Uiso H411 0.8686 0.2895 0.3273 0.0600 1.0000 Uiso H51 1.0494 0.0902 0.3330 0.0600 1.0000 Uiso H52 0.9583 0.0352 0.2880 0.0600 1.0000 Uiso H1441 0.3009 0.1124 -0.0493 0.0600 1.0000 Uiso H1442 0.4583 0.0959 -0.0361 0.0600 1.0000 Uiso H1443 0.3689 0.0885 0.0078 0.0600 1.0000 Uiso H61 1.1721 0.1553 0.2761 0.0600 1.0000 Uiso H62 1.1713 0.0455 0.2686 0.0600 1.0000 Uiso H1431 0.3403 0.2535 -0.0873 0.0600 1.0000 Uiso H1432 0.4361 0.3304 -0.0576 0.0600 1.0000 Uiso H1433 0.4970 0.2349 -0.0735 0.0600 1.0000 Uiso H1621 0.9030 0.5126 0.0871 0.0600 1.0000 Uiso H1622 0.8737 0.4321 0.1250 0.0600 1.0000 Uiso H1623 0.7529 0.4889 0.0931 0.0600 1.0000 Uiso H1011 0.8199 0.0447 0.0134 0.0600 1.0000 Uiso H1012 0.7898 0.1532 0.0083 0.0600 1.0000 Uiso H911 0.5171 0.3532 0.2615 0.0600 1.0000 Uiso H912 0.3587 0.3531 0.2583 0.0600 1.0000 Uiso H431 0.7960 0.1638 0.3737 0.0600 1.0000 Uiso H432 0.8895 0.2328 0.4107 0.0600 1.0000 Uiso H433 0.9483 0.1373 0.3937 0.0600 1.0000 Uiso H1641 0.8495 0.4927 -0.0031 0.0600 1.0000 Uiso H1642 0.7808 0.3997 -0.0272 0.0600 1.0000 Uiso H1643 0.6985 0.4700 0.0021 0.0600 1.0000 Uiso 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 In1 0.0218(3) 0.0211(4) 0.0238(3) 0.0042(4) 0.00437(19) 0.0030(4) Cl1 0.0252(13) 0.0389(15) 0.0367(14) -0.0024(12) 0.003(1) -0.0009(11) Cl2 0.0297(14) 0.0527(18) 0.0411(15) 0.0067(13) 0.0073(11) 0.0105(13) Cl3 0.117(4) 0.094(4) 0.214(5) 0.052(3) 0.098(4) 0.048(3) Cl4 0.065(2) 0.148(4) 0.057(2) -0.006(2) 0.0200(16) -0.028(2) Cl5 0.0391(16) 0.100(3) 0.132(3) -0.035(2) 0.0119(18) 0.0120(18) Cl6 0.093(3) 0.074(2) 0.0512(19) 0.0077(17) -0.0042(17) -0.0048(19) Cl7 0.077(3) 0.081(3) 0.118(3) 0.029(2) -0.010(2) -0.015(2) Cl8 0.073(3) 0.123(3) 0.067(2) -0.008(2) -0.0051(17) -0.008(2) N1 0.026(4) 0.037(5) 0.030(4) 0.011(4) 0.003(3) 0.006(3) N4 0.046(5) 0.060(6) 0.026(4) -0.002(4) 0.004(4) 0.009(5) N7 0.048(5) 0.018(4) 0.026(4) 0.009(3) 0.022(4) 0.026(4) O18 0.021(3) 0.053(4) 0.034(3) 0.008(3) 0.001(2) -0.001(3) C2 0.019(5) 0.075(9) 0.042(6) 0.021(6) 0.016(4) 0.027(6) C3 0.031(6) 0.036(6) 0.041(6) 0.015(5) -0.002(4) -0.002(5) C5 0.019(5) 0.045(7) 0.055(7) -0.011(5) -0.003(4) 0.003(5) C6 0.030(6) 0.029(6) 0.039(6) -0.002(4) 0.001(4) 0.001(4) C8 0.034(6) 0.026(6) 0.047(6) 0.005(4) 0.015(5) 0.003(4) C9 0.033(6) 0.039(6) 0.034(5) 0.000(5) 0.001(4) -0.006(5) C11 0.026(5) 0.051(7) 0.044(6) 0.015(5) 0.015(4) 0.002(5) C12 0.024(5) 0.047(6) 0.023(5) 0.004(4) 0.006(4) -0.006(4) C13 0.011(4) 0.052(6) 0.031(5) 0.001(5) 0.006(4) -0.010(4) C14 0.022(4) 0.075(8) 0.024(4) 0.004(6) -0.001(3) 0.019(6) C15 0.042(6) 0.045(6) 0.022(5) 0.006(4) 0.005(5) -0.007(5) C16 0.036(6) 0.029(6) 0.039(6) -0.006(4) 0.023(5) -0.012(5) C17 0.020(4) 0.053(7) 0.021(4) 0.014(6) -0.003(3) 0.000(6) C41 0.038(5) 0.026(5) 0.036(5) 0.007(5) 0.002(4) 0.011(5) C42 0.078(8) 0.027(6) 0.029(5) -0.011(5) -0.007(5) 0.002(6) C43 0.074(8) 0.095(9) 0.013(4) 0.010(5) 0.017(5) 0.027(7) C71 0.039(6) 0.035(6) 0.053(6) 0.012(5) 0.024(5) 0.011(5) C72 0.052(7) 0.040(7) 0.055(6) 0.000(5) 0.032(5) 0.003(5) C73 0.021(5) 0.089(9) 0.060(7) -0.017(6) 0.015(5) 0.006(6) C81 0.050(8) 0.062(8) 0.070(8) -0.011(6) 0.032(6) -0.005(6) C91 0.031(7) 0.128(12) 0.041(7) -0.000(8) 0.008(5) -0.002(7) C101 0.074(9) 0.054(9) 0.086(11) -0.014(6) 0.003(7) 0.011(7) C141 0.027(6) 0.060(9) 0.050(7) 0.010(6) 0.001(5) -0.009(5) C142 0.033(5) 0.138(13) 0.048(6) -0.021(9) 0.003(4) -0.009(9) C143 0.038(6) 0.167(15) 0.026(5) -0.00(1) -0.021(4) -0.02(1) C144 0.099(11) 0.082(11) 0.051(8) -0.002(7) -0.033(7) -0.023(8) C161 0.032(6) 0.043(6) 0.034(5) -0.003(5) 0.014(4) -0.011(5) C162 0.073(8) 0.055(7) 0.025(5) -0.004(5) 0.005(5) -0.027(6) C163 0.043(6) 0.045(7) 0.081(8) 0.018(6) 0.039(6) -0.004(5) C164 0.066(9) 0.074(9) 0.034(6) 0.024(6) 0.001(6) -0.022(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 In1 . Cl1 . 2.439(2) yes In1 . Cl2 . 2.489(3) yes In1 . N1 . 2.271(8) yes In1 . N4 . 2.366(7) yes In1 . N7 . 2.401(7) yes In1 . O18 . 2.076(5) yes Cl3 . C81 . 1.775(13) yes Cl4 . C81 . 1.767(11) yes Cl5 . C91 . 1.726(16) yes Cl6 . C91 . 1.763(13) yes Cl7 . C101 . 1.761(15) yes Cl8 . C101 . 1.711(14) yes N1 . C2 . 1.423(12) yes N1 . C9 . 1.521(12) yes N1 . C11 . 1.506(12) yes N4 . C3 . 1.508(12) yes N4 . C5 . 1.458(12) yes N4 . C41 . 1.556(12) yes N7 . C6 . 1.499(11) yes N7 . C8 . 1.520(13) yes N7 . C71 . 1.473(11) yes O18 . C17 . 1.385(9) yes C2 . C3 . 1.489(16) yes C2 . H21 . 0.993(11) no C2 . H22 . 0.98(1) no C3 . H31 . 0.991(9) no C3 . H32 . 0.99(1) no C5 . C6 . 1.570(13) yes C5 . H51 . 1.00(1) no C5 . H52 . 0.99(1) no C6 . H61 . 0.986(9) no C6 . H62 . 0.99(1) no C8 . C9 . 1.507(14) yes C8 . H81 . 0.991(9) no C8 . H82 . 1.006(9) no C9 . H91 . 0.989(9) no C9 . H92 . 1.01(1) no C11 . C12 . 1.519(12) yes C11 . H111 . 0.99(1) no C11 . H112 . 1.00(1) no C12 . C13 . 1.393(13) yes C12 . C17 . 1.405(13) yes C13 . C14 . 1.382(13) yes C13 . H131 . 0.990(9) no C14 . C15 . 1.412(14) yes C14 . C141 . 1.547(14) yes C15 . C16 . 1.392(14) yes C15 . H151 . 0.984(9) no C16 . C17 . 1.388(13) yes C16 . C161 . 1.600(12) yes C41 . C42 . 1.493(13) yes C41 . C43 . 1.531(13) yes C41 . H411 . 1.001(9) no C42 . H421 . 0.99(1) no C42 . H422 . 0.99(1) no C42 . H423 . 1.00(1) no C43 . H431 . 0.980(13) no C43 . H432 . 0.989(11) no C43 . H433 . 1.003(11) no C71 . C72 . 1.474(14) yes C71 . C73 . 1.574(15) yes C71 . H711 . 1.00(1) no C72 . H721 . 0.995(9) no C72 . H722 . 1.01(1) no C72 . H723 . 0.985(11) no C73 . H731 . 0.99(1) no C73 . H732 . 0.997(11) no C73 . H733 . 1.007(12) no C81 . H811 . 0.999(13) no C81 . H812 . 0.994(12) no C91 . H911 . 0.989(11) no C91 . H912 . 1.000(12) no C101 . H1011 . 0.973(15) no C101 . H1012 . 1.017(12) no C141 . C142 . 1.505(15) yes C141 . C143 . 1.508(14) yes C141 . C144 . 1.518(18) yes C142 . H1421 . 1.00(1) no C142 . H1422 . 0.966(17) no C142 . H1423 . 0.997(13) no C143 . H1431 . 0.99(1) no C143 . H1432 . 1.002(19) no C143 . H1433 . 0.973(13) no C144 . H1441 . 0.991(12) no C144 . H1442 . 1.010(17) no C144 . H1443 . 0.990(13) no C161 . C162 . 1.513(14) yes C161 . C163 . 1.492(14) yes C161 . C164 . 1.497(15) yes C162 . H1621 . 0.988(11) no C162 . H1622 . 0.99(1) no C162 . H1623 . 0.992(12) no C163 . H1631 . 1.01(1) no C163 . H1632 . 0.980(12) no C163 . H1633 . 0.983(13) no C164 . H1641 . 0.995(11) no C164 . H1642 . 0.984(13) no C164 . H1643 . 0.993(14) 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 . In1 . Cl2 . 95.52(9) yes Cl1 . In1 . N1 . 166.12(19) yes Cl2 . In1 . N1 . 97.70(19) yes Cl1 . In1 . N4 . 106.8(2) yes Cl2 . In1 . N4 . 88.0(2) yes N1 . In1 . N4 . 78.0(3) yes Cl1 . In1 . N7 . 89.2(2) yes Cl2 . In1 . N7 . 166.94(18) yes N1 . In1 . N7 . 78.8(3) yes N4 . In1 . N7 . 79.0(3) yes Cl1 . In1 . O18 . 91.36(17) yes Cl2 . In1 . O18 . 90.45(17) yes N1 . In1 . O18 . 84.3(2) yes N4 . In1 . O18 . 161.8(2) yes N7 . In1 . O18 . 101.6(2) yes In1 . N1 . C2 . 109.6(6) yes In1 . N1 . C9 . 103.9(5) yes C2 . N1 . C9 . 114.6(8) yes In1 . N1 . C11 . 112.5(6) yes C2 . N1 . C11 . 107.1(7) yes C9 . N1 . C11 . 109.3(7) yes In1 . N4 . C3 . 101.7(5) yes In1 . N4 . C5 . 108.0(5) yes C3 . N4 . C5 . 109.4(8) yes In1 . N4 . C41 . 114.9(6) yes C3 . N4 . C41 . 108.2(7) yes C5 . N4 . C41 . 113.9(7) yes In1 . N7 . C6 . 100.8(5) yes In1 . N7 . C8 . 106.1(5) yes C6 . N7 . C8 . 111.0(7) yes In1 . N7 . C71 . 114.6(5) yes C6 . N7 . C71 . 111.7(8) yes C8 . N7 . C71 . 111.9(7) yes In1 . O18 . C17 . 131.8(5) yes N1 . C2 . C3 . 119.1(10) yes N1 . C2 . H21 . 107.3(8) no C3 . C2 . H21 . 106.5(9) no N1 . C2 . H22 . 107.2(8) no C3 . C2 . H22 . 106.8(9) no H21 . C2 . H22 . 109.7(12) no N4 . C3 . C2 . 111.5(8) yes N4 . C3 . H31 . 108.6(8) no C2 . C3 . H31 . 109.6(9) no N4 . C3 . H32 . 108.4(8) no C2 . C3 . H32 . 109.4(8) no H31 . C3 . H32 . 109.3(9) no N4 . C5 . C6 . 115.2(8) yes N4 . C5 . H51 . 109.1(8) no C6 . C5 . H51 . 106.7(8) no N4 . C5 . H52 . 109.3(8) no C6 . C5 . H52 . 107.7(9) no H51 . C5 . H52 . 108.8(10) no N7 . C6 . C5 . 112.6(8) yes N7 . C6 . H61 . 108.5(8) no C5 . C6 . H61 . 108.2(8) no N7 . C6 . H62 . 108.7(8) no C5 . C6 . H62 . 108.7(9) no H61 . C6 . H62 . 110.2(9) no N7 . C8 . C9 . 114.5(7) yes N7 . C8 . H81 . 109.1(8) no C9 . C8 . H81 . 109.0(8) no N7 . C8 . H82 . 107.9(8) no C9 . C8 . H82 . 108.1(8) no H81 . C8 . H82 . 108.2(8) no N1 . C9 . C8 . 112.2(7) yes N1 . C9 . H91 . 109.3(8) no C8 . C9 . H91 . 109.2(8) no N1 . C9 . H92 . 108.6(8) no C8 . C9 . H92 . 109.2(8) no H91 . C9 . H92 . 108.3(8) no N1 . C11 . C12 . 118.0(7) yes N1 . C11 . H111 . 107.2(8) no C12 . C11 . H111 . 107.3(9) no N1 . C11 . H112 . 107.8(8) no C12 . C11 . H112 . 107.1(8) no H111 . C11 . H112 . 109.2(8) no C11 . C12 . C13 . 114.3(8) yes C11 . C12 . C17 . 125.7(8) yes C13 . C12 . C17 . 119.5(8) yes C12 . C13 . C14 . 121.5(8) yes C12 . C13 . H131 . 119.3(9) no C14 . C13 . H131 . 119.2(9) no C13 . C14 . C15 . 118.3(8) yes C13 . C14 . C141 . 120.8(10) yes C15 . C14 . C141 . 120.8(9) yes C14 . C15 . C16 . 120.9(9) yes C14 . C15 . H151 . 119.5(9) no C16 . C15 . H151 . 119.6(9) no C15 . C16 . C17 . 119.8(8) yes C15 . C16 . C161 . 117.6(9) yes C17 . C16 . C161 . 122.3(9) yes O18 . C17 . C12 . 121.8(8) yes O18 . C17 . C16 . 118.3(9) yes C12 . C17 . C16 . 119.9(8) yes N4 . C41 . C42 . 112.1(7) yes N4 . C41 . C43 . 110.2(8) yes C42 . C41 . C43 . 112.8(8) yes N4 . C41 . H411 . 108.3(7) no C42 . C41 . H411 . 104.3(8) no C43 . C41 . H411 . 108.8(7) no C41 . C42 . H421 . 109.8(9) no C41 . C42 . H422 . 109.0(9) no H421 . C42 . H422 . 110.0(9) no C41 . C42 . H423 . 109.7(9) no H421 . C42 . H423 . 109.3(10) no H422 . C42 . H423 . 109.0(10) no C41 . C43 . H431 . 110.0(8) no C41 . C43 . H432 . 110.1(11) no H431 . C43 . H432 . 110.4(10) no C41 . C43 . H433 . 108.6(8) no H431 . C43 . H433 . 109.2(13) no H432 . C43 . H433 . 108.5(10) no N7 . C71 . C72 . 113.2(8) yes N7 . C71 . C73 . 110.9(7) yes C72 . C71 . C73 . 110.7(8) yes N7 . C71 . H711 . 106.2(8) no C72 . C71 . H711 . 108.5(8) no C73 . C71 . H711 . 107.0(9) no C71 . C72 . H721 . 110.8(10) no C71 . C72 . H722 . 109.7(8) no H721 . C72 . H722 . 107.7(10) no C71 . C72 . H723 . 110.7(9) no H721 . C72 . H723 . 109.4(9) no H722 . C72 . H723 . 108.5(10) no C71 . C73 . H731 . 111.1(11) no C71 . C73 . H732 . 111.4(9) no H731 . C73 . H732 . 108.9(10) no C71 . C73 . H733 . 109.5(8) no H731 . C73 . H733 . 108.2(10) no H732 . C73 . H733 . 107.6(12) no Cl3 . C81 . Cl4 . 108.6(6) yes Cl3 . C81 . H811 . 109.5(9) no Cl4 . C81 . H811 . 110.1(9) no Cl3 . C81 . H812 . 109.7(9) no Cl4 . C81 . H812 . 110.6(9) no H811 . C81 . H812 . 108.4(10) no Cl5 . C91 . Cl6 . 109.7(7) yes Cl5 . C91 . H911 . 109.0(11) no Cl6 . C91 . H911 . 111.0(10) no Cl5 . C91 . H912 . 108.1(11) no Cl6 . C91 . H912 . 110.2(10) no H911 . C91 . H912 . 108.8(11) no Cl7 . C101 . Cl8 . 110.2(8) yes Cl7 . C101 . H1011 . 111.1(10) no Cl8 . C101 . H1011 . 110.2(10) no Cl7 . C101 . H1012 . 108.7(10) no Cl8 . C101 . H1012 . 107.8(10) no H1011 . C101 . H1012 . 108.6(14) no C14 . C141 . C142 . 107.7(9) yes C14 . C141 . C143 . 112.0(7) yes C142 . C141 . C143 . 111.9(10) yes C14 . C141 . C144 . 110.2(10) yes C142 . C141 . C144 . 111.3(11) yes C143 . C141 . C144 . 103.8(11) yes C141 . C142 . H1421 . 108.9(10) no C141 . C142 . H1422 . 109.9(10) no H1421 . C142 . H1422 . 110.2(14) no C141 . C142 . H1423 . 109.1(13) no H1421 . C142 . H1423 . 107.8(11) no H1422 . C142 . H1423 . 110.9(11) no C141 . C143 . H1431 . 109.7(11) no C141 . C143 . H1432 . 107.5(10) no H1431 . C143 . H1432 . 108.7(15) no C141 . C143 . H1433 . 109.9(13) no H1431 . C143 . H1433 . 111.1(13) no H1432 . C143 . H1433 . 109.9(13) no C141 . C144 . H1441 . 111.3(12) no C141 . C144 . H1442 . 109.3(12) no H1441 . C144 . H1442 . 107.7(13) no C141 . C144 . H1443 . 111.1(12) no H1441 . C144 . H1443 . 109.4(14) no H1442 . C144 . H1443 . 107.9(13) no C16 . C161 . C162 . 109.0(7) yes C16 . C161 . C163 . 109.3(8) yes C162 . C161 . C163 . 110.0(9) yes C16 . C161 . C164 . 110.1(8) yes C162 . C161 . C164 . 108.5(10) yes C163 . C161 . C164 . 109.9(8) yes C161 . C162 . H1621 . 109.1(8) no C161 . C162 . H1622 . 109.6(10) no H1621 . C162 . H1622 . 109.6(10) no C161 . C162 . H1623 . 109.8(9) no H1621 . C162 . H1623 . 109.5(11) no H1622 . C162 . H1623 . 109.2(9) no C161 . C163 . H1631 . 107.9(10) no C161 . C163 . H1632 . 110.2(9) no H1631 . C163 . H1632 . 109.0(12) no C161 . C163 . H1633 . 110.1(10) no H1631 . C163 . H1633 . 108.7(9) no H1632 . C163 . H1633 . 110.9(11) no C161 . C164 . H1641 . 108.7(10) no C161 . C164 . H1642 . 110.3(11) no H1641 . C164 . H1642 . 109.5(11) no C161 . C164 . H1643 . 109.8(9) no H1641 . C164 . H1643 . 108.8(12) no H1642 . C164 . H1643 . 109.7(11) no #===end data_Compound_13c # Local code str83 _chemical_name_systematic ; [Tl(L-c)] ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _cell_length_a 9.140(3) _cell_angle_alpha 90 _cell_length_b 16.921(5) _cell_angle_beta 93.939(6) _cell_length_c 15.533(2) _cell_angle_gamma 90 _cell_volume 2396.6(5) _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' 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 '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 57.7997 0.0030 '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' 'Tl ' -3.5560 9.6590 27.5446 0.6551 19.1584 8.7075 15.5380 1.9635 5.5259 45.8149 13.1746 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum 'C23 H40 N3 O Tl' _chemical_formula_moiety 'C23 H40 N3 O Tl' _chemical_compound_source ; TlOEt + HL-c ; _chemical_formula_weight 578.96 _cell_measurement_reflns_used 11733 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.60 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1138.32 _exptl_absorpt_coefficient_mu 6.76 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; refined from delta-F (Walker & Stuart , 1983) ; _exptl_absorpt_correction_T_min 0.08 _exptl_absorpt_correction_T_max 0.09 _diffrn_measurement_device_type ; Enraf-nonius DIP2000 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 11733 _reflns_number_total 4718 _diffrn_reflns_av_R_equivalents 0.06 _diffrn_measured_fraction_theta_max 0.943 _reflns_number_gt 4097 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _refine_diff_density_min -0.60 _refine_diff_density_max 0.70 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 4097 _refine_ls_number_parameters 254 _refine_ls_extinction_coef 185.7(75) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _refine_ls_R_factor_gt 0.0201 _refine_ls_wR_factor_ref 0.0241 _refine_ls_goodness_of_fit_ref 1.0540 _refine_ls_shift/su_max 0.0022 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 0.980 0.466E-010.811 ; _computing_data_collection ; DIP2000 software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' loop_ _atom_site_label _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 Tl1 0.839303(9) -0.257670(5) 0.071306(6) 0.0239 1.0000 Uani N1 0.63808(19) -0.1429(1) 0.05521(12) 0.0201 1.0000 Uani N4 0.6548(2) -0.26390(13) -0.08100(14) 0.0275 1.0000 Uani N7 0.8962(2) -0.14799(12) -0.04779(14) 0.0287 1.0000 Uani O18 0.91010(17) -0.16465(9) 0.18321(11) 0.0258 1.0000 Uani C2 0.5076(2) -0.18005(13) 0.01201(15) 0.0241 1.0000 Uani C3 0.5270(3) -0.21094(15) -0.07860(16) 0.0286 1.0000 Uani C5 0.7561(3) -0.24314(15) -0.1468(2) 0.0339 1.0000 Uani C6 0.8231(3) -0.16089(16) -0.13486(17) 0.0334 1.0000 Uani C8 0.8491(3) -0.07462(14) -0.00674(16) 0.0269 1.0000 Uani C9 0.6866(3) -0.07239(13) 0.00851(15) 0.0245 1.0000 Uani C11 0.6070(2) -0.12615(13) 0.14581(15) 0.0230 1.0000 Uani C12 0.7136(2) -0.07440(13) 0.19716(14) 0.0219 1.0000 Uani C13 0.6602(2) -0.00585(13) 0.23470(15) 0.0224 1.0000 Uani C14 0.7477(2) 0.04225(13) 0.28892(14) 0.0218 1.0000 Uani C15 0.8949(2) 0.01955(13) 0.30293(15) 0.0238 1.0000 Uani C16 0.9536(2) -0.04781(13) 0.26937(15) 0.0220 1.0000 Uani C17 0.8618(2) -0.09880(13) 0.21459(14) 0.0215 1.0000 Uani C41 0.6102(3) -0.34656(16) -0.0889(2) 0.0398 1.0000 Uani C71 1.0575(3) -0.14842(18) -0.0507(2) 0.0405 1.0000 Uani C141 0.6914(3) 0.11664(13) 0.33228(14) 0.0237 1.0000 Uani C142 0.7572(3) 0.19014(15) 0.29164(19) 0.0375 1.0000 Uani C143 0.7380(3) 0.11620(17) 0.42903(17) 0.0381 1.0000 Uani C144 0.5245(3) 0.12272(14) 0.32251(17) 0.0307 1.0000 Uani C161 1.1146(2) -0.07066(13) 0.29271(15) 0.0235 1.0000 Uani C162 1.1197(3) -0.14976(14) 0.34173(16) 0.0281 1.0000 Uani C163 1.1955(3) -0.00928(15) 0.35150(19) 0.0348 1.0000 Uani C164 1.1983(3) -0.07911(16) 0.21127(18) 0.0348 1.0000 Uani H21 0.4799 -0.2256 0.0475 0.0600 1.0000 Uiso H22 0.4269 -0.1410 0.0083 0.0600 1.0000 Uiso H31 0.5409 -0.1646 -0.1169 0.0600 1.0000 Uiso H32 0.4370 -0.2394 -0.0994 0.0600 1.0000 Uiso H51 0.8355 -0.2832 -0.1444 0.0600 1.0000 Uiso H52 0.7010 -0.2458 -0.2041 0.0600 1.0000 Uiso H61 0.8969 -0.1549 -0.1783 0.0600 1.0000 Uiso H62 0.7447 -0.1220 -0.1450 0.0600 1.0000 Uiso H81 0.9072 -0.0682 0.0486 0.0600 1.0000 Uiso H82 0.8709 -0.0300 -0.0459 0.0600 1.0000 Uiso H91 0.6676 -0.0250 0.0438 0.0600 1.0000 Uiso H92 0.6290 -0.0692 -0.0472 0.0600 1.0000 Uiso H111 0.6060 -0.1789 0.1757 0.0600 1.0000 Uiso H112 0.5090 -0.1027 0.1455 0.0600 1.0000 Uiso H131 0.5552 0.0072 0.2236 0.0600 1.0000 Uiso H151 0.9607 0.0534 0.3397 0.0600 1.0000 Uiso H411 0.6979 -0.3802 -0.0903 0.0600 1.0000 Uiso H412 0.5466 -0.3537 -0.1424 0.0600 1.0000 Uiso H413 0.5547 -0.3609 -0.0384 0.0600 1.0000 Uiso H711 1.1035 -0.1398 0.0084 0.0600 1.0000 Uiso H712 1.0904 -0.2003 -0.0723 0.0600 1.0000 Uiso H713 1.0877 -0.1060 -0.0892 0.0600 1.0000 Uiso H1421 0.7212 0.2378 0.3194 0.0600 1.0000 Uiso H1422 0.8654 0.1874 0.2998 0.0600 1.0000 Uiso H1423 0.7271 0.1907 0.2292 0.0600 1.0000 Uiso H1431 0.7008 0.1641 0.4560 0.0600 1.0000 Uiso H1432 0.8464 0.1147 0.4367 0.0600 1.0000 Uiso H1433 0.6970 0.0686 0.4555 0.0600 1.0000 Uiso H1441 0.4927 0.1711 0.3524 0.0600 1.0000 Uiso H1442 0.4816 0.0757 0.3505 0.0600 1.0000 Uiso H1443 0.4909 0.1244 0.2615 0.0600 1.0000 Uiso H1621 1.2226 -0.1639 0.3565 0.0600 1.0000 Uiso H1622 1.0669 -0.1433 0.3947 0.0600 1.0000 Uiso H1623 1.0713 -0.1904 0.3044 0.0600 1.0000 Uiso H1631 1.2977 -0.0264 0.3653 0.0600 1.0000 Uiso H1632 1.1448 -0.0043 0.4060 0.0600 1.0000 Uiso H1633 1.1943 0.0424 0.3219 0.0600 1.0000 Uiso H1641 1.3017 -0.0934 0.2275 0.0600 1.0000 Uiso H1642 1.1963 -0.0273 0.1806 0.0600 1.0000 Uiso H1643 1.1522 -0.1197 0.1734 0.0600 1.0000 Uiso 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 Tl1 0.02495(7) 0.01790(7) 0.02801(8) -0.00331(3) -0.00445(4) 0.00331(3) N1 0.0197(9) 0.0215(9) 0.0190(9) -0.0010(6) 0.0010(7) -0.0024(6) N4 0.0276(11) 0.0276(11) 0.0276(12) -0.0093(8) 0.0028(9) -0.0040(7) N7 0.024(1) 0.0342(11) 0.0283(11) -0.0075(8) 0.0058(8) -0.0076(8) O18 0.0244(8) 0.0266(8) 0.0259(9) -0.0057(6) -0.0016(6) 0.0037(6) C2 0.0193(11) 0.0267(11) 0.0260(12) -0.0030(8) 0.0001(8) -0.0024(8) C3 0.0235(12) 0.0343(13) 0.0273(13) -0.0069(9) -0.0037(9) -0.0023(9) C5 0.0314(13) 0.0393(14) 0.0313(16) -0.0114(9) 0.0050(11) -0.005(1) C6 0.0344(14) 0.0428(14) 0.0241(13) -0.005(1) 0.009(1) -0.010(1) C8 0.0302(12) 0.0260(11) 0.0246(12) -0.0016(8) 0.0037(9) -0.0092(9) C9 0.0291(12) 0.020(1) 0.0239(12) 0.0018(8) -0.0020(9) 0.0011(8) C11 0.0207(11) 0.0278(11) 0.0209(12) -0.0041(8) 0.0040(8) -0.0009(8) C12 0.0214(11) 0.024(1) 0.0198(12) -0.0007(8) 0.0009(9) -0.0018(8) C13 0.0201(11) 0.0261(11) 0.0209(11) 0.0027(8) 0.0020(8) 0.0031(8) C14 0.0218(11) 0.021(1) 0.0224(12) 0.0006(8) 0.0008(9) 0.0005(8) C15 0.0229(11) 0.0234(11) 0.0246(12) -0.0009(8) -0.0017(9) -0.0001(8) C16 0.016(1) 0.026(1) 0.0239(12) 0.0022(8) -0.0014(8) 0.0015(7) C17 0.0226(11) 0.023(1) 0.0186(11) 0.0020(8) -0.0009(8) 0.0026(8) C41 0.0412(15) 0.0343(14) 0.0441(17) -0.0122(11) 0.0052(12) -0.0081(11) C71 0.0257(13) 0.0506(16) 0.0464(17) -0.0170(12) 0.0116(11) -0.0091(11) C141 0.0256(12) 0.0236(11) 0.0212(12) -0.0014(8) -0.0028(9) 0.0037(8) C142 0.0376(15) 0.0250(12) 0.0501(17) 0.003(1) 0.0037(12) -0.002(1) C143 0.0445(16) 0.0453(16) 0.0239(14) -0.007(1) -0.0015(11) 0.0140(12) C144 0.0261(12) 0.0281(12) 0.0378(15) -0.0082(9) 0.001(1) 0.0034(9) C161 0.0182(11) 0.023(1) 0.0288(13) 0.0010(8) -0.0010(9) -0.0004(8) C162 0.0244(12) 0.0287(12) 0.0308(13) 0.0033(9) -0.0010(9) 0.0019(8) C163 0.0203(11) 0.0342(13) 0.0484(16) -0.0021(11) -0.008(1) -0.0016(9) C164 0.0246(13) 0.0403(14) 0.0399(16) 0.0060(11) 0.0060(11) 0.002(1) 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 Tl1 . N1 . 2.6744(18) yes Tl1 . N4 . 2.811(2) yes Tl1 . N7 . 2.696(2) yes Tl1 . O18 . 2.4006(16) yes N1 . C2 . 1.469(3) yes N1 . C9 . 1.480(3) yes N1 . C11 . 1.482(3) yes N4 . C3 . 1.475(3) yes N4 . C5 . 1.469(3) yes N4 . C41 . 1.460(3) yes N7 . C6 . 1.483(3) yes N7 . C8 . 1.473(3) yes N7 . C71 . 1.478(3) yes O18 . C17 . 1.305(3) yes C2 . C3 . 1.523(3) yes C2 . H21 . 0.991(2) no C2 . H22 . 0.989(2) no C3 . H31 . 0.997(3) no C3 . H32 . 0.988(2) no C5 . C6 . 1.527(3) yes C5 . H51 . 0.992(3) no C5 . H52 . 0.992(3) no C6 . H61 . 0.992(2) no C6 . H62 . 0.978(3) no C8 . C9 . 1.520(3) yes C8 . H81 . 0.985(2) no C8 . H82 . 0.998(2) no C9 . H91 . 0.994(2) no C9 . H92 . 0.984(2) no C11 . C12 . 1.498(3) yes C11 . H111 . 1.006(2) no C11 . H112 . 0.980(2) no C12 . C13 . 1.401(3) yes C12 . C17 . 1.424(3) yes C13 . C14 . 1.385(3) yes C13 . H131 . 0.988(2) no C14 . C15 . 1.401(3) yes C14 . C141 . 1.533(3) yes C15 . C16 . 1.377(3) yes C15 . H151 . 0.984(2) no C16 . C17 . 1.440(3) yes C16 . C161 . 1.541(3) yes C41 . H411 . 0.984(3) no C41 . H412 . 0.989(3) no C41 . H413 . 0.993(3) no C71 . H711 . 0.994(3) no C71 . H712 . 0.993(3) no C71 . H713 . 0.986(3) no C141 . C142 . 1.536(3) yes C141 . C143 . 1.534(3) yes C141 . C144 . 1.526(3) yes C142 . H1421 . 0.982(3) no C142 . H1422 . 0.990(3) no C142 . H1423 . 0.990(3) no C143 . H1431 . 0.984(3) no C143 . H1432 . 0.990(3) no C143 . H1433 . 0.990(3) no C144 . H1441 . 0.994(2) no C144 . H1442 . 0.999(3) no C144 . H1443 . 0.976(3) no C161 . C162 . 1.539(3) yes C161 . C163 . 1.538(3) yes C161 . C164 . 1.529(4) yes C162 . H1621 . 0.982(2) no C162 . H1622 . 0.988(3) no C162 . H1623 . 0.985(2) no C163 . H1631 . 0.988(3) no C163 . H1632 . 0.996(3) no C163 . H1633 . 0.987(3) no C164 . H1641 . 0.991(3) no C164 . H1642 . 0.998(3) no C164 . H1643 . 0.980(3) 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 . Tl1 . N4 . 65.15(6) yes N1 . Tl1 . N7 . 66.41(6) yes N4 . Tl1 . N7 . 65.24(6) yes N1 . Tl1 . O18 . 74.99(5) yes N4 . Tl1 . O18 . 138.61(6) yes N7 . Tl1 . O18 . 89.45(6) yes Tl1 . N1 . C2 . 105.28(12) yes Tl1 . N1 . C9 . 113.81(13) yes C2 . N1 . C9 . 112.47(17) yes Tl1 . N1 . C11 . 103.03(12) yes C2 . N1 . C11 . 108.27(17) yes C9 . N1 . C11 . 113.23(17) yes Tl1 . N4 . C3 . 112.73(14) yes Tl1 . N4 . C5 . 101.93(16) yes C3 . N4 . C5 . 114.2(2) yes Tl1 . N4 . C41 . 104.74(16) yes C3 . N4 . C41 . 111.6(2) yes C5 . N4 . C41 . 110.9(2) yes Tl1 . N7 . C6 . 115.37(14) yes Tl1 . N7 . C8 . 101.97(14) yes C6 . N7 . C8 . 113.1(2) yes Tl1 . N7 . C71 . 104.91(17) yes C6 . N7 . C71 . 111.1(2) yes C8 . N7 . C71 . 109.80(19) yes Tl1 . O18 . C17 . 138.48(14) yes N1 . C2 . C3 . 115.28(19) yes N1 . C2 . H21 . 108.06(19) no C3 . C2 . H21 . 107.3(2) no N1 . C2 . H22 . 108.64(19) no C3 . C2 . H22 . 108.0(2) no H21 . C2 . H22 . 109.5(2) no N4 . C3 . C2 . 111.98(19) yes N4 . C3 . H31 . 109.2(2) no C2 . C3 . H31 . 108.0(2) no N4 . C3 . H32 . 109.8(2) no C2 . C3 . H32 . 108.8(2) no H31 . C3 . H32 . 109.0(2) no N4 . C5 . C6 . 113.6(2) yes N4 . C5 . H51 . 107.7(3) no C6 . C5 . H51 . 109.4(2) no N4 . C5 . H52 . 107.9(2) no C6 . C5 . H52 . 109.0(3) no H51 . C5 . H52 . 109.1(2) no N7 . C6 . C5 . 113.4(2) yes N7 . C6 . H61 . 108.7(2) no C5 . C6 . H61 . 107.2(2) no N7 . C6 . H62 . 109.1(2) no C5 . C6 . H62 . 108.1(2) no H61 . C6 . H62 . 110.3(3) no N7 . C8 . C9 . 113.93(18) yes N7 . C8 . H81 . 108.4(2) no C9 . C8 . H81 . 109.6(2) no N7 . C8 . H82 . 107.3(2) no C9 . C8 . H82 . 108.3(2) no H81 . C8 . H82 . 109.2(2) no N1 . C9 . C8 . 112.66(18) yes N1 . C9 . H91 . 108.1(2) no C8 . C9 . H91 . 108.4(2) no N1 . C9 . H92 . 108.40(19) no C8 . C9 . H92 . 109.5(2) no H91 . C9 . H92 . 109.7(2) no N1 . C11 . C12 . 117.23(18) yes N1 . C11 . H111 . 106.09(18) no C12 . C11 . H111 . 107.4(2) no N1 . C11 . H112 . 107.9(2) no C12 . C11 . H112 . 109.1(2) no H111 . C11 . H112 . 109.0(2) no C11 . C12 . C13 . 118.2(2) yes C11 . C12 . C17 . 120.4(2) yes C13 . C12 . C17 . 121.0(2) yes C12 . C13 . C14 . 122.4(2) yes C12 . C13 . H131 . 118.3(2) no C14 . C13 . H131 . 119.2(2) no C13 . C14 . C15 . 116.2(2) yes C13 . C14 . C141 . 123.5(2) yes C15 . C14 . C141 . 120.30(19) yes C14 . C15 . C16 . 124.2(2) yes C14 . C15 . H151 . 118.2(2) no C16 . C15 . H151 . 117.6(2) no C15 . C16 . C17 . 119.5(2) yes C15 . C16 . C161 . 120.6(2) yes C17 . C16 . C161 . 119.81(19) yes O18 . C17 . C12 . 121.2(2) yes O18 . C17 . C16 . 122.24(19) yes C12 . C17 . C16 . 116.5(2) yes N4 . C41 . H411 . 109.5(2) no N4 . C41 . H412 . 109.4(3) no H411 . C41 . H412 . 110.0(3) no N4 . C41 . H413 . 108.9(2) no H411 . C41 . H413 . 109.7(3) no H412 . C41 . H413 . 109.3(3) no N7 . C71 . H711 . 109.3(2) no N7 . C71 . H712 . 109.9(2) no H711 . C71 . H712 . 108.9(3) no N7 . C71 . H713 . 109.6(3) no H711 . C71 . H713 . 109.5(3) no H712 . C71 . H713 . 109.6(3) no C14 . C141 . C142 . 109.4(2) yes C14 . C141 . C143 . 110.33(19) yes C142 . C141 . C143 . 108.5(2) yes C14 . C141 . C144 . 112.03(18) yes C142 . C141 . C144 . 108.75(19) yes C143 . C141 . C144 . 107.8(2) yes C141 . C142 . H1421 . 109.4(2) no C141 . C142 . H1422 . 109.0(2) no H1421 . C142 . H1422 . 110.1(3) no C141 . C142 . H1423 . 108.7(2) no H1421 . C142 . H1423 . 110.1(3) no H1422 . C142 . H1423 . 109.5(3) no C141 . C143 . H1431 . 109.4(2) no C141 . C143 . H1432 . 109.1(2) no H1431 . C143 . H1432 . 110.0(3) no C141 . C143 . H1433 . 108.9(2) no H1431 . C143 . H1433 . 110.0(3) no H1432 . C143 . H1433 . 109.5(3) no C141 . C144 . H1441 . 109.3(2) no C141 . C144 . H1442 . 108.8(2) no H1441 . C144 . H1442 . 108.4(2) no C141 . C144 . H1443 . 110.1(2) no H1441 . C144 . H1443 . 110.3(2) no H1442 . C144 . H1443 . 109.9(2) no C16 . C161 . C162 . 109.29(18) yes C16 . C161 . C163 . 112.50(19) yes C162 . C161 . C163 . 107.3(2) yes C16 . C161 . C164 . 110.65(19) yes C162 . C161 . C164 . 109.2(2) yes C163 . C161 . C164 . 107.9(2) yes C161 . C162 . H1621 . 108.9(2) no C161 . C162 . H1622 . 108.4(2) no H1621 . C162 . H1622 . 110.3(2) no C161 . C162 . H1623 . 108.6(2) no H1621 . C162 . H1623 . 110.6(2) no H1622 . C162 . H1623 . 110.1(2) no C161 . C163 . H1631 . 109.9(2) no C161 . C163 . H1632 . 109.2(2) no H1631 . C163 . H1632 . 109.2(3) no C161 . C163 . H1633 . 109.4(2) no H1631 . C163 . H1633 . 109.9(2) no H1632 . C163 . H1633 . 109.2(3) no C161 . C164 . H1641 . 109.6(2) no C161 . C164 . H1642 . 108.6(2) no H1641 . C164 . H1642 . 108.7(2) no C161 . C164 . H1643 . 110.1(2) no H1641 . C164 . H1643 . 110.2(3) no H1642 . C164 . H1643 . 109.6(3) no #=== end data_Compound_13b # Local code str104 _chemical_name_systematic ; [Tl(L-b)] ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _cell_length_a 9.5230(4) _cell_angle_alpha 79.328(3) _cell_length_b 11.1850(3) _cell_angle_beta 74.964(2) _cell_length_c 13.6500(6) _cell_angle_gamma 78.089(3) _cell_volume 1360.5 _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 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 '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 57.7997 0.0030 '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' 'Tl ' -3.5560 9.6590 27.5446 0.6551 19.1584 8.7075 15.5380 1.9635 5.5259 45.8149 13.1746 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum 'C27 H48 N3 O Tl' _chemical_formula_moiety 'C27 H48 N3 O Tl' _chemical_compound_source ; HL-b + TlOEt ; _chemical_formula_weight 635.07 _cell_measurement_reflns_used 15076 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourless' _exptl_crystal_size_min 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.55 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 633.14 _exptl_absorpt_coefficient_mu 5.96 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; refined from delta-F (Walker & Stuart , 1983) ; _exptl_absorpt_correction_T_min 0.18 _exptl_absorpt_correction_T_max 0.23 _diffrn_measurement_device_type ; Enraf-nonius DIP2000 ; _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 15076 _reflns_number_total 5135 _diffrn_reflns_av_R_equivalents 0.03 _diffrn_measured_fraction_theta_max 0.904 _reflns_number_gt 4847 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _refine_diff_density_min -0.67 _refine_diff_density_max 0.94 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 4847 _refine_ls_number_parameters 181 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0361 _refine_ls_goodness_of_fit_ref 0.7733 _refine_ls_shift/su_max 0.0019 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w = 1/(0.00 *F +0.00 *\s^2^(F ) + 0.00 ) ; _refine_ls_extinction_method 'None' _computing_data_collection ; DIP2000 software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SHELXS86 (Sheldrick, 1986)' loop_ _atom_site_label _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 Tl1 0.38850(2) 0.141762(18) 0.828190(15) 0.0189 1.0000 Uani N1 0.4960(4) 0.2688(4) 0.9262(3) 0.0201 1.0000 Uani N4 0.5669(4) 0.3227(4) 0.6969(3) 0.0216 1.0000 Uani N7 0.2565(4) 0.3879(4) 0.8216(3) 0.0205 1.0000 Uani O18 0.2472(4) 0.1122(3) 1.0032(3) 0.0248 1.0000 Uani C2 0.6445(6) 0.2839(5) 0.8634(4) 0.0251 1.0000 Uani C3 0.6459(6) 0.3653(5) 0.7599(4) 0.0248 1.0000 Uani C5 0.4542(6) 0.4200(5) 0.6599(4) 0.0241 1.0000 Uani C6 0.3324(6) 0.4774(5) 0.7434(4) 0.0244 1.0000 Uani C8 0.2511(5) 0.4062(5) 0.9270(4) 0.0224 1.0000 Uani C9 0.4028(6) 0.3863(5) 0.9519(4) 0.0236 1.0000 Uani C11 0.5162(6) 0.1753(5) 1.0189(4) 0.0257 1.0000 Uani C12 0.3824(5) 0.1699(5) 1.1051(4) 0.0205 1.0000 Uani C13 0.3906(6) 0.1942(5) 1.2003(4) 0.0244 1.0000 Uani C14 0.2730(6) 0.1907(5) 1.2852(4) 0.0254 1.0000 Uani C15 0.1430(6) 0.1628(5) 1.2705(4) 0.0250 1.0000 Uani C16 0.1294(5) 0.1361(5) 1.1785(4) 0.0213 1.0000 Uani C172 0.0080(6) -0.0233(5) 1.1382(4) 0.0285 1.0000 Uani C41 0.6616(6) 0.2579(5) 0.6118(4) 0.0283 1.0000 Uani C174 -0.1366(6) 0.1088(7) 1.2686(5) 0.0388 1.0000 Uani C43 0.7470 0.3408 0.5240 0.0391 1.0000 Uani C71 0.1062 0.3812 0.8107 0.0253 1.0000 Uani C72 0.1142 0.3479 0.7056 0.0321 1.0000 Uani C73 -0.0070 0.4979 0.8290 0.0341 1.0000 Uani C141 0.2797 0.2195 1.3895 0.0368 1.0000 Uani C142 0.1758 0.3455 1.4083 0.0612 1.0000 Uani C143 0.2197 0.1295 1.4754 0.0778 1.0000 Uani C144 0.4309 0.2404 1.3918 0.0663 1.0000 Uani C171 -0.0171 0.1060 1.1688 0.0247 1.0000 Uani C17 0.2518 0.1389 1.0921 0.0205 1.0000 Uani C173 -0.0771 0.2011 1.0858 0.0317 1.0000 Uani C42 0.7668 0.1487 0.6503 0.0347 1.0000 Uani H21 0.6939 0.3213 0.9028 0.0600 1.0000 Uiso H22 0.7006 0.2012 0.8505 0.0600 1.0000 Uiso H31 0.5986 0.4504 0.7723 0.0600 1.0000 Uiso H32 0.7496 0.3654 0.7217 0.0600 1.0000 Uiso H51 0.5049 0.4868 0.6162 0.0600 1.0000 Uiso H52 0.4073 0.3835 0.6183 0.0600 1.0000 Uiso H61 0.3768 0.5251 0.7782 0.0600 1.0000 Uiso H62 0.2581 0.5338 0.7102 0.0600 1.0000 Uiso H81 0.2020 0.4917 0.9365 0.0600 1.0000 Uiso H82 0.1925 0.3474 0.9754 0.0600 1.0000 Uiso H91 0.3883 0.3877 1.0262 0.0600 1.0000 Uiso H92 0.4546 0.4546 0.9128 0.0600 1.0000 Uiso H111 0.5948 0.1954 1.0453 0.0600 1.0000 Uiso H112 0.5480 0.0928 0.9963 0.0600 1.0000 Uiso H131 0.4835 0.2146 1.2073 0.0600 1.0000 Uiso H151 0.0564 0.1622 1.3292 0.0600 1.0000 Uiso H1721 -0.0865 -0.0417 1.1322 0.0600 1.0000 Uiso H1722 0.0463 -0.0850 1.1911 0.0600 1.0000 Uiso H1723 0.0803 -0.0266 1.0716 0.0600 1.0000 Uiso H411 0.5923 0.2283 0.5825 0.0600 1.0000 Uiso H1741 -0.2276 0.0888 1.2578 0.0600 1.0000 Uiso H1742 -0.1018 0.0472 1.3230 0.0600 1.0000 Uiso H1743 -0.1577 0.1921 1.2893 0.0600 1.0000 Uiso H431 0.8074 0.2908 0.4704 0.0600 1.0000 Uiso H432 0.8121 0.3788 0.5507 0.0600 1.0000 Uiso H433 0.6765 0.4065 0.4944 0.0600 1.0000 Uiso H711 0.0711 0.3156 0.8656 0.0600 1.0000 Uiso H721 0.0138 0.3439 0.6997 0.0600 1.0000 Uiso H722 0.1559 0.4116 0.6516 0.0600 1.0000 Uiso H723 0.1779 0.2668 0.6975 0.0600 1.0000 Uiso H731 -0.1030 0.4859 0.8204 0.0600 1.0000 Uiso H732 -0.0184 0.5152 0.8994 0.0600 1.0000 Uiso H733 0.0270 0.5682 0.7790 0.0600 1.0000 Uiso H1421 0.1780 0.3664 1.4752 0.0600 1.0000 Uiso H1422 0.2101 0.4112 1.3531 0.0600 1.0000 Uiso H1423 0.0738 0.3386 1.4084 0.0600 1.0000 Uiso H1431 0.2265 0.1520 1.5406 0.0600 1.0000 Uiso H1432 0.2771 0.0461 1.4665 0.0600 1.0000 Uiso H1433 0.1152 0.1297 1.4767 0.0600 1.0000 Uiso H1441 0.4289 0.2585 1.4605 0.0600 1.0000 Uiso H1442 0.5041 0.1654 1.3766 0.0600 1.0000 Uiso H1443 0.4585 0.3110 1.3396 0.0600 1.0000 Uiso H1731 -0.1710 0.1817 1.0796 0.0600 1.0000 Uiso H1732 -0.0944 0.2848 1.1053 0.0600 1.0000 Uiso H1733 -0.0043 0.1978 1.0194 0.0600 1.0000 Uiso H421 0.8286 0.1072 0.5918 0.0600 1.0000 Uiso H422 0.8307 0.1780 0.6844 0.0600 1.0000 Uiso H423 0.7096 0.0898 0.6998 0.0600 1.0000 Uiso 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 Tl1 0.0189(1) 0.02011(11) 0.0181(1) -0.00241(7) -0.00417(7) -0.00448(7) N1 0.0177(19) 0.024(2) 0.019(2) 0.0012(16) -0.0051(16) -0.0052(17) N4 0.019(2) 0.024(2) 0.021(2) -0.0001(17) -0.0060(16) -0.0013(17) N7 0.0182(19) 0.023(2) 0.019(2) -0.0035(16) -0.0040(16) -0.0011(17) O18 0.0198(17) 0.034(2) 0.0220(18) -0.0027(15) -0.0048(14) -0.0082(15) C2 0.020(2) 0.032(3) 0.022(2) 0.001(2) -0.004(2) -0.008(2) C3 0.024(2) 0.031(3) 0.021(2) 0.001(2) -0.005(2) -0.011(2) C5 0.021(2) 0.026(3) 0.022(2) 0.002(2) -0.006(2) -0.002(2) C6 0.024(3) 0.021(3) 0.025(3) 0.000(2) -0.005(2) -0.002(2) C8 0.022(2) 0.025(3) 0.019(2) -0.0025(19) -0.0050(19) -0.001(2) C9 0.025(3) 0.024(3) 0.023(2) -0.003(2) -0.005(2) -0.006(2) C11 0.019(2) 0.035(3) 0.024(3) 0.002(2) -0.009(2) -0.006(2) C12 0.019(2) 0.021(3) 0.019(2) 0.0030(19) -0.0046(19) -0.004(2) C13 0.026(3) 0.025(3) 0.024(3) 0.001(2) -0.011(2) -0.006(2) C14 0.027(3) 0.028(3) 0.023(3) -0.002(2) -0.008(2) -0.006(2) C15 0.022(2) 0.027(3) 0.024(3) 0.002(2) -0.004(2) -0.005(2) C16 0.021(2) 0.021(3) 0.023(2) 0.0022(19) -0.0071(19) -0.006(2) C172 0.026(3) 0.027(3) 0.035(3) 0.001(2) -0.012(2) -0.008(2) C41 0.024(3) 0.035(3) 0.024(3) -0.007(2) -0.002(2) -0.002(2) C174 0.024(3) 0.060(4) 0.036(3) -0.008(3) -0.001(2) -0.019(3) C43 0.0343 0.0431 0.0299 0.0012 -0.0031 0.0043 C71 0.0233 0.0296 0.0243 -0.0027 -0.0071 -0.0057 C72 0.0303 0.0384 0.0285 -0.0075 -0.0081 -0.0034 C73 0.0173 0.0458 0.0348 -0.0058 -0.0045 0.0031 C141 0.0361 0.0543 0.0249 -0.0092 -0.0060 -0.0166 C142 0.0962 0.0556 0.0403 -0.0212 -0.0160 -0.0184 C143 0.1424 0.0863 0.0282 0.0028 -0.0268 -0.0717 C144 0.0649 0.1043 0.0416 -0.0170 -0.0142 -0.0324 C171 0.0202 0.0292 0.0239 -0.0009 -0.0045 -0.0054 C17 0.0193 0.0185 0.0232 -0.0010 -0.0067 -0.0015 C173 0.0266 0.0309 0.0411 -0.0020 -0.0178 -0.0025 C42 0.0319 0.0322 0.0361 -0.0034 -0.0054 -0.0006 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 Tl1 . O18 . 2.419(3) yes Tl1 . N1 . 2.622(4) yes Tl1 . N4 . 2.948(4) yes Tl1 . N7 . 2.776(4) yes N1 . C2 . 1.477(6) yes N1 . C9 . 1.471(7) yes N1 . C11 . 1.511(6) yes N4 . C3 . 1.472(6) yes N4 . C5 . 1.479(6) yes N4 . C41 . 1.479(7) yes N7 . C6 . 1.471(6) yes N7 . C8 . 1.478(6) yes N7 . C71 . 1.496(4) yes O18 . C17 . 1.316(3) yes C2 . C3 . 1.531(7) yes C2 . H21 . 0.990(5) no C2 . H22 . 0.990(6) no C3 . H31 . 0.990(6) no C3 . H32 . 0.990(5) no C5 . C6 . 1.528(7) yes C5 . H51 . 0.990(5) no C5 . H52 . 0.990(5) no C6 . H61 . 0.990(5) no C6 . H62 . 0.990(5) no C8 . C9 . 1.531(7) yes C8 . H81 . 0.990(5) no C8 . H82 . 0.990(5) no C9 . H91 . 0.990(5) no C9 . H92 . 0.990(5) no C11 . C12 . 1.497(7) yes C11 . H111 . 0.990(5) no C11 . H112 . 0.990(6) no C12 . C13 . 1.400(7) yes C12 . C17 . 1.419(5) yes C13 . C14 . 1.388(7) yes C13 . H131 . 0.990(5) no C14 . C15 . 1.408(7) yes C14 . C141 . 1.537(5) yes C15 . C16 . 1.386(7) yes C15 . H151 . 0.990(5) no C16 . C171 . 1.544(5) yes C16 . C17 . 1.428(5) yes C172 . C171 . 1.533(6) yes C172 . H1721 . 0.990(5) no C172 . H1722 . 0.990(5) no C172 . H1723 . 0.990(6) no C41 . C43 . 1.533(5) yes C41 . C42 . 1.517(6) yes C41 . H411 . 0.990(5) no C174 . C171 . 1.533(6) yes C174 . H1741 . 0.990(6) no C174 . H1742 . 0.990(7) no C174 . H1743 . 0.990(7) no C43 . H431 . 0.990 no C43 . H432 . 0.990 no C43 . H433 . 0.990 no C71 . C72 . 1.526 yes C71 . C73 . 1.526 yes C71 . H711 . 0.990 no C72 . H721 . 0.990 no C72 . H722 . 0.990 no C72 . H723 . 0.990 no C73 . H731 . 0.990 no C73 . H732 . 0.990 no C73 . H733 . 0.990 no C141 . C142 . 1.568 yes C141 . C143 . 1.471 yes C141 . C144 . 1.515 yes C142 . H1421 . 0.990 no C142 . H1422 . 0.990 no C142 . H1423 . 0.990 no C143 . H1431 . 0.990 no C143 . H1432 . 0.990 no C143 . H1433 . 0.990 no C144 . H1441 . 0.990 no C144 . H1442 . 0.990 no C144 . H1443 . 0.990 no C171 . C173 . 1.542 yes C173 . H1731 . 0.990 no C173 . H1732 . 0.990 no C173 . H1733 . 0.990 no C42 . H421 . 0.990 no C42 . H422 . 0.990 no C42 . H423 . 0.990 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 . Tl1 . N4 . 64.83(12) yes N1 . Tl1 . N7 . 66.37(12) yes N4 . Tl1 . N7 . 63.63(12) yes N1 . Tl1 . O18 . 75.41(12) yes N4 . Tl1 . O18 . 137.21(12) yes N7 . Tl1 . O18 . 86.92(12) yes Tl1 . N1 . C2 . 106.1(3) yes Tl1 . N1 . C9 . 115.3(3) yes C2 . N1 . C9 . 113.1(4) yes Tl1 . N1 . C11 . 100.4(3) yes C2 . N1 . C11 . 107.2(4) yes C9 . N1 . C11 . 113.7(4) yes Tl1 . N4 . C3 . 108.5(3) yes Tl1 . N4 . C5 . 102.5(3) yes C3 . N4 . C5 . 113.5(4) yes C3 . N4 . C41 . 115.4(4) yes Tl1 . N4 . C41 . 105.2(3) yes C5 . N4 . C41 . 110.6(4) yes Tl1 . N7 . C6 . 117.2(3) yes Tl1 . N7 . C8 . 99.5(3) yes C6 . N7 . C8 . 112.7(4) yes Tl1 . N7 . C71 . 101.4(2) yes C6 . N7 . C71 . 114.2(3) yes C8 . N7 . C71 . 110.5(3) yes Tl1 . O18 . C17 . 136.7(2) yes N1 . C2 . C3 . 114.5(4) yes N1 . C2 . H21 . 108.2(4) no C3 . C2 . H21 . 108.2(4) no N1 . C2 . H22 . 108.2(4) no C3 . C2 . H22 . 108.2(5) no H21 . C2 . H22 . 109.5(5) no N4 . C3 . C2 . 113.0(4) yes N4 . C3 . H31 . 108.6(4) no C2 . C3 . H31 . 108.6(5) no N4 . C3 . H32 . 108.6(4) no C2 . C3 . H32 . 108.6(5) no H31 . C3 . H32 . 109.5(5) no N4 . C5 . C6 . 115.4(4) yes N4 . C5 . H51 . 108.0(4) no C6 . C5 . H51 . 108.0(5) no N4 . C5 . H52 . 108.0(5) no C6 . C5 . H52 . 108.0(4) no H51 . C5 . H52 . 109.5(5) no N7 . C6 . C5 . 114.6(4) yes N7 . C6 . H61 . 108.2(4) no C5 . C6 . H61 . 108.2(4) no N7 . C6 . H62 . 108.2(4) no C5 . C6 . H62 . 108.2(4) no H61 . C6 . H62 . 109.5(5) no N7 . C8 . C9 . 114.0(4) yes N7 . C8 . H81 . 108.3(4) no C9 . C8 . H81 . 108.3(4) no N7 . C8 . H82 . 108.3(4) no C9 . C8 . H82 . 108.3(4) no H81 . C8 . H82 . 109.5(5) no N1 . C9 . C8 . 113.6(4) yes N1 . C9 . H91 . 108.4(4) no C8 . C9 . H91 . 108.4(4) no N1 . C9 . H92 . 108.4(4) no C8 . C9 . H92 . 108.4(4) no H91 . C9 . H92 . 109.5(5) no N1 . C11 . C12 . 115.6(4) yes N1 . C11 . H111 . 107.9(4) no C12 . C11 . H111 . 107.9(5) no N1 . C11 . H112 . 107.9(4) no C12 . C11 . H112 . 107.9(5) no H111 . C11 . H112 . 109.5(5) no C11 . C12 . C13 . 117.9(4) yes C11 . C12 . C17 . 121.5(4) yes C13 . C12 . C17 . 120.6(4) yes C12 . C13 . C14 . 122.3(5) yes C12 . C13 . H131 . 118.8(5) no C14 . C13 . H131 . 118.8(5) no C13 . C14 . C15 . 116.4(5) yes C13 . C14 . C141 . 122.8(4) yes C15 . C14 . C141 . 120.8(4) yes C14 . C15 . C16 . 123.8(5) yes C14 . C15 . H151 . 118.1(5) no C16 . C15 . H151 . 118.1(5) no C15 . C16 . C171 . 120.6(4) yes C15 . C16 . C17 . 119.2(4) yes C171 . C16 . C17 . 120.2(3) yes C171 . C172 . H1721 . 109.5(5) no C171 . C172 . H1722 . 109.5(4) no H1721 . C172 . H1722 . 109.5(5) no C171 . C172 . H1723 . 109.5(4) no H1721 . C172 . H1723 . 109.5(5) no H1722 . C172 . H1723 . 109.5(5) no N4 . C41 . C43 . 114.4(4) yes N4 . C41 . C42 . 111.3(4) yes C43 . C41 . C42 . 110.1(3) yes N4 . C41 . H411 . 104.9(4) no C43 . C41 . H411 . 106.1(4) no C42 . C41 . H411 . 109.7(5) no C171 . C174 . H1741 . 109.5(5) no C171 . C174 . H1742 . 109.5(5) no H1741 . C174 . H1742 . 109.5(6) no C171 . C174 . H1743 . 109.5(5) no H1741 . C174 . H1743 . 109.5(6) no H1742 . C174 . H1743 . 109.5(6) no C41 . C43 . H431 . 109.5(2) no C41 . C43 . H432 . 109.5(2) no H431 . C43 . H432 . 109.475 no C41 . C43 . H433 . 109.5(2) no H431 . C43 . H433 . 109.476 no H432 . C43 . H433 . 109.476 no N7 . C71 . C72 . 110.53(15) yes N7 . C71 . C73 . 114.55(16) yes C72 . C71 . C73 . 109.587 yes N7 . C71 . H711 . 105.18(16) no C72 . C71 . H711 . 110.597 no C73 . C71 . H711 . 106.210 no C71 . C72 . H721 . 109.467 no C71 . C72 . H722 . 109.467 no H721 . C72 . H722 . 109.476 no C71 . C72 . H723 . 109.467 no H721 . C72 . H723 . 109.476 no H722 . C72 . H723 . 109.476 no C71 . C73 . H731 . 109.467 no C71 . C73 . H732 . 109.467 no H731 . C73 . H732 . 109.476 no C71 . C73 . H733 . 109.467 no H731 . C73 . H733 . 109.475 no H732 . C73 . H733 . 109.476 no C14 . C141 . C142 . 107.7(2) yes C14 . C141 . C143 . 112.6(2) yes C142 . C141 . C143 . 104.973 yes C14 . C141 . C144 . 112.88(19) yes C142 . C141 . C144 . 104.839 yes C143 . C141 . C144 . 113.017 yes C141 . C142 . H1421 . 109.467 no C141 . C142 . H1422 . 109.467 no H1421 . C142 . H1422 . 109.476 no C141 . C142 . H1423 . 109.467 no H1421 . C142 . H1423 . 109.476 no H1422 . C142 . H1423 . 109.476 no C141 . C143 . H1431 . 109.467 no C141 . C143 . H1432 . 109.467 no H1431 . C143 . H1432 . 109.476 no C141 . C143 . H1433 . 109.467 no H1431 . C143 . H1433 . 109.476 no H1432 . C143 . H1433 . 109.476 no C141 . C144 . H1441 . 109.467 no C141 . C144 . H1442 . 109.467 no H1441 . C144 . H1442 . 109.476 no C141 . C144 . H1443 . 109.467 no H1441 . C144 . H1443 . 109.476 no H1442 . C144 . H1443 . 109.476 no C16 . C171 . C172 . 110.1(3) yes C16 . C171 . C174 . 113.0(3) yes C172 . C171 . C174 . 107.4(3) yes C16 . C171 . C173 . 109.50(18) yes C172 . C171 . C173 . 108.9(2) yes C174 . C171 . C173 . 107.7(3) yes O18 . C17 . C12 . 120.1(2) yes O18 . C17 . C16 . 122.3(2) yes C12 . C17 . C16 . 117.7(3) yes C171 . C173 . H1731 . 109.467 no C171 . C173 . H1732 . 109.467 no H1731 . C173 . H1732 . 109.476 no C171 . C173 . H1733 . 109.467 no H1731 . C173 . H1733 . 109.476 no H1732 . C173 . H1733 . 109.476 no C41 . C42 . H421 . 109.5(2) no C41 . C42 . H422 . 109.5(2) no H421 . C42 . H422 . 109.476 no C41 . C42 . H423 . 109.5(2) no H421 . C42 . H423 . 109.476 no H422 . C42 . H423 . 109.476 no #=== end