# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1818 data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-04-17 _audit_update_record ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal 'J.Chem.Soc., Dalton' _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; #<< references text Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_tly # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C45 H33 N6 Tl3' _chemical_formula_moiety ? _chemical_formula_weight 1270.95 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 9.495(2) _cell_length_b 15.506(3) _cell_length_c 26.159(5) _cell_angle_alpha 90.00000 _cell_angle_beta 96.587(4) _cell_angle_gamma 90.00000 _cell_volume 3826.0(13) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.206 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 3638 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 12.646 _exptl_crystal_description wedge _exptl_crystal_size_max .25 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min 0.262 _exptl_absorpt_correction_T_max 0.617 _diffrn_reflns_number 42807 _reflns_number_total 6654 _reflns_Friedel_coverage 0 _reflns_number_gt 4072 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 24.88 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .072 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .064 _refine_ls_wR_factor_ref .071 _refine_ls_goodness_of_fit_ref 1.742 _refine_ls_number_reflns 4072 _refine_ls_number_parameters 233 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .027 _refine_diff_density_min -2.695 _refine_diff_density_max 3.919 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 1508(200) _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 180 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 132 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 24 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Tl ? 0 12 -3.556 9.659 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Tl1 .17114(10) .21234(6) .12398(4) .0291(6) Uani ? ? 1.00000 ? ? Tl2 -.16663(10) .21492(6) .20381(4) .0282(6) Uani ? ? 1.00000 ? ? Tl3 .11904(10) -.01499(6) .20031(4) .0283(5) Uani ? ? 1.00000 ? ? N11 .196(2) .1766(12) .2261(7) .026(5) Uiso ? ? 1.00000 ? ? N12 .0750(17) .1391(11) .2418(7) .018(4) Uiso ? ? 1.00000 ? ? C13 .081(2) .1540(13) .2918(9) .015(5) Uiso ? ? 1.00000 ? ? C131 -.036(2) .1286(14) .3212(9) .020(6) Uiso ? ? 1.00000 ? ? C132 -.143(2) .0703(14) .2982(9) .028(6) Uiso ? ? 1.00000 ? ? C133 -.259(2) .0526(15) .3268(10) .030(6) Uiso ? ? 1.00000 ? ? C134 -.271(3) .0841(16) .3745(10) .034(6) Uiso ? ? 1.00000 ? ? C135 -.168(3) .1394(16) .3947(10) .040(7) Uiso ? ? 1.00000 ? ? C136 -.052(2) .1604(14) .3699(9) .024(6) Uiso ? ? 1.00000 ? ? C14 .206(2) .1983(13) .3094(9) .022(6) Uiso ? ? 1.00000 ? ? C15 .271(2) .2120(14) .2676(9) .020(5) Uiso ? ? 1.00000 ? ? C151 .401(2) .2624(13) .2631(9) .021(6) Uiso ? ? 1.00000 ? ? C152 .422(2) .3096(14) .2211(9) .026(6) Uiso ? ? 1.00000 ? ? C153 .550(3) .3595(16) .2198(10) .036(7) Uiso ? ? 1.00000 ? ? C154 .645(2) .3649(14) .2624(9) .026(6) Uiso ? ? 1.00000 ? ? C155 .628(3) .3180(15) .3043(10) .032(6) Uiso ? ? 1.00000 ? ? C156 .506(3) .2658(15) .3045(10) .034(7) Uiso ? ? 1.00000 ? ? N21 -.0864(19) .1391(11) .1171(7) .025(5) Uiso ? ? 1.00000 ? ? N22 -.0089(18) .0613(11) .1179(7) .023(5) Uiso ? ? 1.00000 ? ? C23 -.061(2) .0156(15) .0781(9) .026(6) Uiso ? ? 1.00000 ? ? C231 -.006(2) -.0708(14) .0673(9) .021(6) Uiso ? ? 1.00000 ? ? C232 .139(2) -.0905(14) .0815(9) .024(6) Uiso ? ? 1.00000 ? ? C233 .192(3) -.1738(16) .0690(10) .038(7) Uiso ? ? 1.00000 ? ? C234 .101(3) -.2327(15) .0448(10) .033(7) Uiso ? ? 1.00000 ? ? C235 -.038(3) -.2137(17) .0318(10) .039(7) Uiso ? ? 1.00000 ? ? C236 -.092(3) -.1338(16) .0437(10) .033(7) Uiso ? ? 1.00000 ? ? C24 -.176(2) .0586(14) .0519(9) .025(6) Uiso ? ? 1.00000 ? ? C25 -.188(2) .1341(15) .0765(9) .026(6) Uiso ? ? 1.00000 ? ? C251 -.296(2) .2039(14) .0659(9) .025(6) Uiso ? ? 1.00000 ? ? C252 -.278(2) .2848(15) .0863(9) .028(6) Uiso ? ? 1.00000 ? ? C253 -.383(3) .3480(16) .0787(10) .038(7) Uiso ? ? 1.00000 ? ? C254 -.509(3) .3274(17) .0515(11) .039(7) Uiso ? ? 1.00000 ? ? C255 -.527(3) .2458(15) .0301(10) .031(6) Uiso ? ? 1.00000 ? ? C256 -.423(2) .1874(14) .0358(10) .028(6) Uiso ? ? 1.00000 ? ? N31 .0480(19) .3481(12) .1576(7) .027(5) Uiso ? ? 1.00000 ? ? N32 .014(2) .3486(12) .2073(8) .029(5) Uiso ? ? 1.00000 ? ? C33 .052(3) .4239(16) .2272(10) .034(7) Uiso ? ? 1.00000 ? ? C331 .021(2) .4460(14) .2824(9) .024(6) Uiso ? ? 1.00000 ? ? C332 -.007(2) .3826(14) .3173(9) .020(5) Uiso ? ? 1.00000 ? ? C333 -.034(3) .4047(16) .3640(10) .034(7) Uiso ? ? 1.00000 ? ? C334 -.029(3) .4946(16) .3806(10) .037(7) Uiso ? ? 1.00000 ? ? C335 -.008(3) .5559(16) .3466(10) .038(7) Uiso ? ? 1.00000 ? ? C336 .018(2) .5349(14) .2978(9) .028(6) Uiso ? ? 1.00000 ? ? C34 .115(2) .4718(12) .1947(8) .011(5) Uiso ? ? 1.00000 ? ? C35 .111(2) .4274(13) .1494(9) .019(5) Uiso ? ? 1.00000 ? ? C351 .153(2) .4494(13) .0995(9) .019(5) Uiso ? ? 1.00000 ? ? C352 .095(2) .4111(15) .0538(10) .028(6) Uiso ? ? 1.00000 ? ? C353 .129(2) .4323(14) .0072(9) .025(6) Uiso ? ? 1.00000 ? ? C354 .230(3) .4936(16) .0046(10) .037(7) Uiso ? ? 1.00000 ? ? C355 .294(2) .5341(15) .0475(10) .028(6) Uiso ? ? 1.00000 ? ? C356 .259(2) .5099(14) .0948(9) .026(6) Uiso ? ? 1.00000 ? ? H132 -.13522 .04375 .26433 .03400 Uiso ? ? 1.00000 ? ? H133 -.33398 .01523 .31098 .03700 Uiso ? ? 1.00000 ? ? H134 -.34925 .06769 .39290 .04100 Uiso ? ? 1.00000 ? ? H135 -.17626 .16401 .42851 .05100 Uiso ? ? 1.00000 ? ? H136 .02096 .19846 .38701 .03300 Uiso ? ? 1.00000 ? ? H14 .23820 .21538 .34487 .02600 Uiso ? ? 1.00000 ? ? H152 .35042 .31021 .19159 .03500 Uiso ? ? 1.00000 ? ? H153 .56772 .38958 .18832 .04400 Uiso ? ? 1.00000 ? ? H154 .72759 .40254 .26262 .03000 Uiso ? ? 1.00000 ? ? H155 .69725 .32049 .33445 .03800 Uiso ? ? 1.00000 ? ? H156 .49489 .23078 .33444 .04200 Uiso ? ? 1.00000 ? ? H232 .20181 -.04702 .09865 .03200 Uiso ? ? 1.00000 ? ? H233 .29061 -.18832 .07992 .04800 Uiso ? ? 1.00000 ? ? H234 .13594 -.28841 .03503 .04300 Uiso ? ? 1.00000 ? ? H235 -.10021 -.25684 .01382 .04900 Uiso ? ? 1.00000 ? ? H236 -.19193 -.12167 .03502 .04300 Uiso ? ? 1.00000 ? ? H24 -.23513 .03809 .02115 .03000 Uiso ? ? 1.00000 ? ? H252 -.18973 .29849 .10745 .03400 Uiso ? ? 1.00000 ? ? H253 -.36648 .40580 .09180 .04600 Uiso ? ? 1.00000 ? ? H254 -.58506 .37009 .04738 .04800 Uiso ? ? 1.00000 ? ? H255 -.61772 .23151 .01043 .03700 Uiso ? ? 1.00000 ? ? H256 -.43587 .13232 .01818 .03400 Uiso ? ? 1.00000 ? ? H332 -.00623 .32209 .30726 .02600 Uiso ? ? 1.00000 ? ? H333 -.05859 .36035 .38742 .04400 Uiso ? ? 1.00000 ? ? H334 -.04010 .50904 .41620 .04300 Uiso ? ? 1.00000 ? ? H335 -.01015 .61530 .35674 .04800 Uiso ? ? 1.00000 ? ? H336 .03555 .57969 .27327 .03200 Uiso ? ? 1.00000 ? ? H34 .15822 .52820 .20211 .01400 Uiso ? ? 1.00000 ? ? H352 .02388 .36640 .05615 .03400 Uiso ? ? 1.00000 ? ? H353 .08386 .40409 -.02326 .03200 Uiso ? ? 1.00000 ? ? H354 .25427 .51078 -.02955 .04700 Uiso ? ? 1.00000 ? ? H355 .36605 .57852 .04516 .03600 Uiso ? ? 1.00000 ? ? H356 .30884 .53510 .12606 .03300 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Tl1 .0270(6) .0206(5) .0410(8) -.0025(4) .0088(5) -.0027(5) Tl2 .0230(5) .0202(5) .0419(8) .0016(4) .0060(5) -.0002(5) Tl3 .0246(5) .0169(5) .0435(7) .0006(4) .0048(5) .0000(5) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Tl1 Tl2 . . 4.0230(16) ? Tl1 Tl3 . . 4.1090(15) ? Tl1 N11 . . 2.71(2) ? Tl1 N21 . . 2.683(18) ? Tl1 N22 . . 2.893(17) ? Tl1 N31 . . 2.608(19) ? Tl1 N32 . . 3.49(2) ? Tl1 C35 . . 3.46(2) ? Tl1 H152 . . 2.7637(10) ? Tl2 Tl3 . . 4.4867(14) ? Tl2 N11 . . 3.478(18) ? Tl2 N12 . . 2.667(16) ? Tl2 C13 . . 3.24(2) ? Tl2 C131 . . 3.45(2) ? Tl2 C132 . . 3.32(2) ? Tl2 N21 . . 2.74(2) ? Tl2 C252 . . 3.32(2) ? Tl2 N31 . . 3.232(19) ? Tl2 N32 . . 2.686(19) ? Tl2 H252 . . 2.8203(11) ? Tl2 C154 . '1 455' 3.40(2) ? Tl3 N11 . . 3.115(18) ? Tl3 N12 . . 2.676(17) ? Tl3 N22 . . 2.630(18) ? Tl3 C23 . . 3.48(2) ? Tl3 C232 . . 3.35(2) ? Tl3 H232 . . 2.9011(12) ? Tl3 C152 . '2 545' 3.46(2) ? Tl3 C153 . '2 545' 3.39(3) ? Tl3 C154 . '2 545' 3.36(2) ? Tl3 C155 . '2 545' 3.49(2) ? Tl3 C331 . '2 545' 3.45(2) ? N11 N12 . . 1.39(3) ? N11 C15 . . 1.34(3) ? N12 C13 . . 1.32(3) ? C13 C131 . . 1.48(3) ? C13 C14 . . 1.40(3) ? C131 C132 . . 1.44(3) ? C131 C136 . . 1.39(3) ? C132 C133 . . 1.43(4) ? C132 H132 . . .99(2) ? C133 C134 . . 1.36(4) ? C133 H133 . . .97(2) ? C134 C135 . . 1.36(3) ? C134 H134 . . .97(3) ? C135 C136 . . 1.37(4) ? C135 H135 . . .97(3) ? C136 H136 . . .98(2) ? C14 C15 . . 1.33(3) ? C14 H14 . . .98(2) ? C15 C151 . . 1.48(3) ? C151 C152 . . 1.35(3) ? C151 C156 . . 1.38(3) ? C152 C153 . . 1.44(3) ? C152 H152 . . .97(2) ? C153 C154 . . 1.35(3) ? C153 H153 . . .98(3) ? C154 C155 . . 1.34(4) ? C154 H154 . . .97(2) ? C155 C156 . . 1.42(3) ? C155 H155 . . .97(2) ? C156 H156 . . .97(3) ? N21 N22 . . 1.41(2) ? N21 C25 . . 1.35(3) ? N22 C23 . . 1.31(3) ? C23 C231 . . 1.48(3) ? C23 C24 . . 1.39(3) ? C231 C232 . . 1.42(3) ? C231 C236 . . 1.37(3) ? C232 C233 . . 1.44(3) ? C232 H232 . . .98(2) ? C233 C234 . . 1.36(3) ? C233 H233 . . .97(2) ? C234 C235 . . 1.36(3) ? C234 H234 . . .97(2) ? C235 C236 . . 1.39(4) ? C235 H235 . . .98(3) ? C236 H236 . . .97(2) ? C24 C25 . . 1.35(3) ? C24 H24 . . .98(2) ? C25 C251 . . 1.50(3) ? C251 C252 . . 1.37(3) ? C251 C256 . . 1.38(3) ? C252 C253 . . 1.39(3) ? C252 H252 . . .98(2) ? C253 C254 . . 1.35(3) ? C253 H253 . . .97(3) ? C254 C255 . . 1.39(4) ? C254 H254 . . .98(3) ? C255 C256 . . 1.33(3) ? C255 H255 . . .98(2) ? C256 H256 . . .97(2) ? N31 N32 . . 1.38(3) ? N31 C35 . . 1.39(3) ? N32 C33 . . 1.31(3) ? C33 C331 . . 1.55(4) ? C33 C34 . . 1.32(3) ? C331 C332 . . 1.39(3) ? C331 C336 . . 1.44(3) ? C332 C333 . . 1.32(4) ? C332 H332 . . .97(2) ? C333 C334 . . 1.46(4) ? C333 H333 . . .97(3) ? C334 C335 . . 1.33(4) ? C334 H334 . . .97(3) ? C335 C336 . . 1.37(4) ? C335 H335 . . .96(3) ? C336 H336 . . .97(2) ? C34 C35 . . 1.37(3) ? C34 H34 . . .978(19) ? C35 C351 . . 1.45(3) ? C351 C352 . . 1.39(3) ? C351 C356 . . 1.39(3) ? C352 C353 . . 1.34(4) ? C352 H352 . . .97(2) ? C353 C354 . . 1.35(3) ? C353 H353 . . .97(2) ? C354 C355 . . 1.37(3) ? C354 H354 . . .99(3) ? C355 C356 . . 1.37(3) ? C355 H355 . . .98(2) ? C356 H356 . . .98(2) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Tl2 Tl1 Tl3 . . . 66.96(3) ? Tl2 Tl1 N11 . . . 58.4(4) ? Tl2 Tl1 N21 . . . 42.7(4) ? Tl2 Tl1 N22 . . . 62.3(4) ? Tl2 Tl1 N31 . . . 53.3(4) ? Tl2 Tl1 N32 . . . 41.1(3) ? Tl2 Tl1 C35 . . . 74.4(4) ? Tl2 Tl1 H152 . . . 97.56(3) ? Tl3 Tl1 N11 . . . 49.3(4) ? Tl3 Tl1 N21 . . . 60.7(4) ? Tl3 Tl1 N22 . . . 39.5(3) ? Tl3 Tl1 N31 . . . 116.4(4) ? Tl3 Tl1 N32 . . . 97.6(3) ? Tl3 Tl1 C35 . . . 134.5(4) ? Tl3 Tl1 H152 . . . 105.05(3) ? N11 Tl1 N21 . . . 87.5(6) ? N11 Tl1 N22 . . . 82.7(5) ? N11 Tl1 N31 . . . 79.9(6) ? N11 Tl1 N32 . . . 60.3(5) ? N11 Tl1 C35 . . . 90.3(5) ? N11 Tl1 H152 . . . 60.3(4) ? N21 Tl1 N22 . . . 29.0(5) ? N21 Tl1 N31 . . . 85.6(6) ? N21 Tl1 N32 . . . 81.2(5) ? N21 Tl1 C35 . . . 104.5(5) ? N21 Tl1 H152 . . . 139.9(4) ? N22 Tl1 N31 . . . 112.7(5) ? N22 Tl1 N32 . . . 103.4(5) ? N22 Tl1 C35 . . . 132.9(5) ? N22 Tl1 H152 . . . 142.8(4) ? N31 Tl1 N32 . . . 20.1(5) ? N31 Tl1 C35 . . . 21.2(5) ? N31 Tl1 H152 . . . 66.9(4) ? N32 Tl1 C35 . . . 37.3(5) ? N32 Tl1 H152 . . . 62.9(3) ? C35 Tl1 H152 . . . 56.7(3) ? Tl1 Tl2 Tl3 . . . 57.44(2) ? Tl1 Tl2 N11 . . . 41.6(3) ? Tl1 Tl2 N12 . . . 59.1(4) ? Tl1 Tl2 C13 . . . 78.9(4) ? Tl1 Tl2 C131 . . . 103.4(4) ? Tl1 Tl2 C132 . . . 112.9(4) ? Tl1 Tl2 N21 . . . 41.6(4) ? Tl1 Tl2 C252 . . . 73.2(4) ? Tl1 Tl2 N31 . . . 40.3(3) ? Tl1 Tl2 N32 . . . 58.7(4) ? Tl1 Tl2 H252 . . . 61.68(3) ? Tl1 Tl2 C154 . . '1 455' 137.0(4) ? Tl3 Tl2 N11 . . . 43.8(3) ? Tl3 Tl2 N12 . . . 33.0(4) ? Tl3 Tl2 C13 . . . 52.5(4) ? Tl3 Tl2 C131 . . . 63.5(4) ? Tl3 Tl2 C132 . . . 59.3(4) ? Tl3 Tl2 N21 . . . 54.3(4) ? Tl3 Tl2 C252 . . . 111.8(4) ? Tl3 Tl2 N31 . . . 95.2(3) ? Tl3 Tl2 N32 . . . 103.2(4) ? Tl3 Tl2 H252 . . . 109.40(3) ? Tl3 Tl2 C154 . . '1 455' 154.4(4) ? N11 Tl2 N12 . . . 21.4(5) ? N11 Tl2 C13 . . . 37.4(5) ? N11 Tl2 C131 . . . 62.4(5) ? N11 Tl2 C132 . . . 77.3(5) ? N11 Tl2 N21 . . . 72.6(5) ? N11 Tl2 C252 . . . 114.6(5) ? N11 Tl2 N31 . . . 61.1(4) ? N11 Tl2 N32 . . . 60.6(5) ? N11 Tl2 H252 . . . 101.7(3) ? N11 Tl2 C154 . . '1 455' 127.0(5) ? N12 Tl2 C13 . . . 23.4(6) ? N12 Tl2 C131 . . . 44.9(5) ? N12 Tl2 C132 . . . 56.2(6) ? N12 Tl2 N21 . . . 79.1(5) ? N12 Tl2 C252 . . . 131.3(6) ? N12 Tl2 N31 . . . 82.5(5) ? N12 Tl2 N32 . . . 79.0(5) ? N12 Tl2 H252 . . . 120.7(4) ? N12 Tl2 C154 . . '1 455' 127.4(5) ? C13 Tl2 C131 . . . 25.3(5) ? C13 Tl2 C132 . . . 45.1(5) ? C13 Tl2 N21 . . . 102.4(5) ? C13 Tl2 C252 . . . 152.0(6) ? C13 Tl2 N31 . . . 90.8(5) ? C13 Tl2 N32 . . . 78.0(5) ? C13 Tl2 H252 . . . 138.2(4) ? C13 Tl2 C154 . . '1 455' 104.8(5) ? C131 Tl2 C132 . . . 24.4(5) ? C131 Tl2 N21 . . . 117.7(5) ? C131 Tl2 C252 . . . 175.2(6) ? C131 Tl2 N31 . . . 113.8(5) ? C131 Tl2 N32 . . . 96.1(5) ? C131 Tl2 H252 . . . 163.3(4) ? C131 Tl2 C154 . . '1 455' 91.0(5) ? C132 Tl2 N21 . . . 108.9(6) ? C132 Tl2 C252 . . . 153.6(6) ? C132 Tl2 N31 . . . 135.9(5) ? C132 Tl2 N32 . . . 120.5(6) ? C132 Tl2 H252 . . . 164.9(4) ? C132 Tl2 C154 . . '1 455' 96.9(6) ? N21 Tl2 C252 . . . 57.5(6) ? N21 Tl2 N31 . . . 73.6(5) ? N21 Tl2 N32 . . . 97.0(6) ? N21 Tl2 H252 . . . 57.1(4) ? N21 Tl2 C154 . . '1 455' 151.2(5) ? C252 Tl2 N31 . . . 66.0(5) ? C252 Tl2 N32 . . . 85.1(6) ? C252 Tl2 H252 . . . 15.8(4) ? C252 Tl2 C154 . . '1 455' 93.8(6) ? N31 Tl2 N32 . . . 24.7(6) ? N31 Tl2 H252 . . . 50.2(3) ? N31 Tl2 C154 . . '1 455' 96.8(5) ? N32 Tl2 H252 . . . 70.1(4) ? N32 Tl2 C154 . . '1 455' 79.8(6) ? H252 Tl2 C154 . . '1 455' 95.6(4) ? Tl1 Tl3 Tl2 . . . 55.60(2) ? Tl1 Tl3 N11 . . . 41.3(4) ? Tl1 Tl3 N12 . . . 57.6(4) ? Tl1 Tl3 N22 . . . 44.4(4) ? Tl1 Tl3 C23 . . . 60.7(4) ? Tl1 Tl3 C232 . . . 80.0(4) ? Tl1 Tl3 H232 . . . 68.96(3) ? Tl1 Tl3 C152 . . '2 545' 172.6(4) ? Tl1 Tl3 C153 . . '2 545' 152.1(4) ? Tl1 Tl3 C154 . . '2 545' 138.8(4) ? Tl1 Tl3 C155 . . '2 545' 137.6(4) ? Tl1 Tl3 C331 . . '2 545' 92.4(4) ? Tl2 Tl3 N11 . . . 50.6(3) ? Tl2 Tl3 N12 . . . 32.8(3) ? Tl2 Tl3 N22 . . . 55.6(4) ? Tl2 Tl3 C23 . . . 71.1(4) ? Tl2 Tl3 C232 . . . 113.3(4) ? Tl2 Tl3 H232 . . . 112.50(3) ? Tl2 Tl3 C152 . . '2 545' 120.2(4) ? Tl2 Tl3 C153 . . '2 545' 96.5(4) ? Tl2 Tl3 C154 . . '2 545' 87.8(4) ? Tl2 Tl3 C155 . . '2 545' 100.7(4) ? Tl2 Tl3 C331 . . '2 545' 136.8(4) ? N11 Tl3 N12 . . . 26.5(5) ? N11 Tl3 N22 . . . 79.8(5) ? N11 Tl3 C23 . . . 98.5(5) ? N11 Tl3 C232 . . . 119.9(5) ? N11 Tl3 H232 . . . 106.3(4) ? N11 Tl3 C152 . . '2 545' 131.4(5) ? N11 Tl3 C153 . . '2 545' 122.0(6) ? N11 Tl3 C154 . . '2 545' 129.1(5) ? N11 Tl3 C155 . . '2 545' 148.9(5) ? N11 Tl3 C331 . . '2 545' 86.2(5) ? N12 Tl3 N22 . . . 81.5(5) ? N12 Tl3 C23 . . . 99.7(5) ? N12 Tl3 C232 . . . 135.8(5) ? N12 Tl3 H232 . . . 126.6(4) ? N12 Tl3 C152 . . '2 545' 115.3(6) ? N12 Tl3 C153 . . '2 545' 98.9(6) ? N12 Tl3 C154 . . '2 545' 102.7(5) ? N12 Tl3 C155 . . '2 545' 122.8(6) ? N12 Tl3 C331 . . '2 545' 107.6(5) ? N22 Tl3 C23 . . . 19.0(5) ? N22 Tl3 C232 . . . 57.7(5) ? N22 Tl3 H232 . . . 58.3(4) ? N22 Tl3 C152 . . '2 545' 140.1(5) ? N22 Tl3 C153 . . '2 545' 123.8(6) ? N22 Tl3 C154 . . '2 545' 101.4(5) ? N22 Tl3 C155 . . '2 545' 93.5(5) ? N22 Tl3 C331 . . '2 545' 122.9(6) ? C23 Tl3 C232 . . . 43.0(5) ? C23 Tl3 H232 . . . 48.5(4) ? C23 Tl3 C152 . . '2 545' 125.1(5) ? C23 Tl3 C153 . . '2 545' 115.2(6) ? C23 Tl3 C154 . . '2 545' 92.1(5) ? C23 Tl3 C155 . . '2 545' 79.1(6) ? C23 Tl3 C331 . . '2 545' 121.3(6) ? C232 Tl3 H232 . . . 16.0(4) ? C232 Tl3 C152 . . '2 545' 107.4(6) ? C232 Tl3 C153 . . '2 545' 116.9(6) ? C232 Tl3 C154 . . '2 545' 101.5(6) ? C232 Tl3 C155 . . '2 545' 79.4(6) ? C232 Tl3 C331 . . '2 545' 84.3(5) ? H232 Tl3 C152 . . '2 545' 118.1(4) ? H232 Tl3 C153 . . '2 545' 131.6(4) ? H232 Tl3 C154 . . '2 545' 117.5(4) ? H232 Tl3 C155 . . '2 545' 95.3(4) ? H232 Tl3 C331 . . '2 545' 73.8(4) ? C152 Tl3 C153 '2 545' . '2 545' 24.3(6) ? C152 Tl3 C154 '2 545' . '2 545' 41.6(5) ? C152 Tl3 C155 '2 545' . '2 545' 46.7(5) ? C152 Tl3 C331 '2 545' . '2 545' 87.9(5) ? C153 Tl3 C154 '2 545' . '2 545' 23.1(6) ? C153 Tl3 C155 '2 545' . '2 545' 39.7(6) ? C153 Tl3 C331 '2 545' . '2 545' 110.5(6) ? C154 Tl3 C155 '2 545' . '2 545' 22.5(6) ? C154 Tl3 C331 '2 545' . '2 545' 128.8(5) ? C155 Tl3 C331 '2 545' . '2 545' 121.8(5) ? Tl1 N11 Tl2 . . . 80.0(4) ? Tl1 N11 Tl3 . . . 89.4(5) ? Tl1 N11 N12 . . . 113.2(12) ? Tl1 N11 C15 . . . 133.7(15) ? Tl2 N11 Tl3 . . . 85.6(4) ? Tl2 N11 N12 . . . 44.4(9) ? Tl2 N11 C15 . . . 119.0(14) ? Tl3 N11 N12 . . . 58.9(9) ? Tl3 N11 C15 . . . 130.9(14) ? N12 N11 C15 . . . 108.0(18) ? Tl2 N12 Tl3 . . . 114.2(6) ? Tl2 N12 N11 . . . 114.2(12) ? Tl2 N12 C13 . . . 103.3(12) ? Tl3 N12 N11 . . . 94.6(11) ? Tl3 N12 C13 . . . 124.4(13) ? N11 N12 C13 . . . 105.9(16) ? Tl2 C13 N12 . . . 53.3(10) ? Tl2 C13 C131 . . . 85.2(11) ? Tl2 C13 C14 . . . 127.5(14) ? N12 C13 C131 . . . 121.1(18) ? N12 C13 C14 . . . 111(2) ? C131 C13 C14 . . . 128(2) ? Tl2 C131 C13 . . . 69.5(11) ? Tl2 C131 C132 . . . 73.0(13) ? Tl2 C131 C136 . . . 127.8(14) ? C13 C131 C132 . . . 119(2) ? C13 C131 C136 . . . 123.4(19) ? C132 C131 C136 . . . 117(2) ? Tl2 C132 C131 . . . 82.5(13) ? Tl2 C132 C133 . . . 121.9(15) ? Tl2 C132 H132 . . . 67.7(13) ? C131 C132 C133 . . . 117(2) ? C131 C132 H132 . . . 121(2) ? C133 C132 H132 . . . 122(2) ? C132 C133 C134 . . . 124(2) ? C132 C133 H133 . . . 117(2) ? C134 C133 H133 . . . 118(2) ? C133 C134 C135 . . . 117(2) ? C133 C134 H134 . . . 121(2) ? C135 C134 H134 . . . 122(3) ? C134 C135 C136 . . . 123(2) ? C134 C135 H135 . . . 118(3) ? C136 C135 H135 . . . 119(2) ? C131 C136 C135 . . . 122(2) ? C131 C136 H136 . . . 119(2) ? C135 C136 H136 . . . 119(2) ? C13 C14 C15 . . . 105(2) ? C13 C14 H14 . . . 127(2) ? C15 C14 H14 . . . 128(2) ? N11 C15 C14 . . . 110(2) ? N11 C15 C151 . . . 121(2) ? C14 C15 C151 . . . 128(2) ? C15 C151 C152 . . . 124(2) ? C15 C151 C156 . . . 119(2) ? C152 C151 C156 . . . 117(2) ? C151 C152 C153 . . . 121(2) ? C151 C152 H152 . . . 120(2) ? C151 C152 Tl3 . . 2 84.6(14) ? C153 C152 H152 . . . 119(2) ? C153 C152 Tl3 . . 2 75.2(14) ? H152 C152 Tl3 . . 2 110.3(15) ? C152 C153 C154 . . . 120(2) ? C152 C153 H153 . . . 120(2) ? C152 C153 Tl3 . . 2 80.5(14) ? C154 C153 H153 . . . 120(2) ? C154 C153 Tl3 . . 2 77.1(15) ? H153 C153 Tl3 . . 2 112.6(17) ? C153 C154 C155 . . . 120(2) ? C153 C154 H154 . . . 120(2) ? C153 C154 Tl2 . . '1 655' 85.6(15) ? C153 C154 Tl3 . . 2 79.7(15) ? C155 C154 H154 . . . 120(2) ? C155 C154 Tl2 . . '1 655' 96.8(15) ? C155 C154 Tl3 . . 2 84.1(15) ? H154 C154 Tl2 . . '1 655' 87.2(14) ? H154 C154 Tl3 . . 2 106.9(15) ? Tl2 C154 Tl3 '1 655' . 2 163.4(7) ? C154 C155 C156 . . . 119(2) ? C154 C155 H155 . . . 120(2) ? C154 C155 Tl3 . . 2 73.4(14) ? C156 C155 H155 . . . 120(2) ? C156 C155 Tl3 . . 2 82.9(14) ? H155 C155 Tl3 . . 2 112.9(17) ? C151 C156 C155 . . . 122(2) ? C151 C156 H156 . . . 119(2) ? C155 C156 H156 . . . 119(2) ? Tl1 N21 Tl2 . . . 95.8(6) ? Tl1 N21 N22 . . . 83.8(11) ? Tl1 N21 C25 . . . 129.7(15) ? Tl2 N21 N22 . . . 123.2(13) ? Tl2 N21 C25 . . . 115.8(14) ? N22 N21 C25 . . . 106.6(17) ? Tl1 N22 Tl3 . . . 96.0(5) ? Tl1 N22 N21 . . . 67.2(10) ? Tl1 N22 C23 . . . 130.5(15) ? Tl3 N22 N21 . . . 126.1(13) ? Tl3 N22 C23 . . . 120.3(14) ? N21 N22 C23 . . . 107.5(17) ? Tl3 C23 N22 . . . 40.7(11) ? Tl3 C23 C231 . . . 84.6(12) ? Tl3 C23 C24 . . . 142.6(17) ? N22 C23 C231 . . . 122(2) ? N22 C23 C24 . . . 110(2) ? C231 C23 C24 . . . 128(2) ? C23 C231 C232 . . . 120.0(19) ? C23 C231 C236 . . . 122(2) ? C232 C231 C236 . . . 118(2) ? Tl3 C232 C231 . . . 90.7(14) ? Tl3 C232 C233 . . . 125.7(16) ? Tl3 C232 H232 . . . 55.2(12) ? C231 C232 C233 . . . 119(2) ? C231 C232 H232 . . . 120(2) ? C233 C232 H232 . . . 121(2) ? C232 C233 C234 . . . 119(2) ? C232 C233 H233 . . . 120(2) ? C234 C233 H233 . . . 121(2) ? C233 C234 C235 . . . 121(2) ? C233 C234 H234 . . . 120(2) ? C235 C234 H234 . . . 119(2) ? C234 C235 C236 . . . 121(2) ? C234 C235 H235 . . . 119(2) ? C236 C235 H235 . . . 120(2) ? C231 C236 C235 . . . 121(2) ? C231 C236 H236 . . . 119(2) ? C235 C236 H236 . . . 120(2) ? C23 C24 C25 . . . 107(2) ? C23 C24 H24 . . . 126(2) ? C25 C24 H24 . . . 127(2) ? N21 C25 C24 . . . 110(2) ? N21 C25 C251 . . . 121(2) ? C24 C25 C251 . . . 129(2) ? C25 C251 C252 . . . 123(2) ? C25 C251 C256 . . . 120(2) ? C252 C251 C256 . . . 117(2) ? Tl2 C252 C251 . . . 94.2(14) ? Tl2 C252 C253 . . . 120.6(17) ? Tl2 C252 H252 . . . 51.8(12) ? C251 C252 C253 . . . 122(2) ? C251 C252 H252 . . . 119(2) ? C253 C252 H252 . . . 119(2) ? C252 C253 C254 . . . 119(2) ? C252 C253 H253 . . . 121(2) ? C254 C253 H253 . . . 120(2) ? C253 C254 C255 . . . 119(2) ? C253 C254 H254 . . . 120(3) ? C255 C254 H254 . . . 121(2) ? C254 C255 C256 . . . 121(2) ? C254 C255 H255 . . . 119(2) ? C256 C255 H255 . . . 120(2) ? C251 C256 C255 . . . 121(2) ? C251 C256 H256 . . . 119(2) ? C255 C256 H256 . . . 119(2) ? Tl1 N31 Tl2 . . . 86.4(5) ? Tl1 N31 N32 . . . 119.1(13) ? Tl1 N31 C35 . . . 116.4(14) ? Tl2 N31 N32 . . . 54.8(10) ? Tl2 N31 C35 . . . 157.0(14) ? N32 N31 C35 . . . 106.9(17) ? Tl1 N32 Tl2 . . . 80.1(5) ? Tl1 N32 N31 . . . 40.8(10) ? Tl1 N32 C33 . . . 132.1(16) ? Tl2 N32 N31 . . . 100.4(12) ? Tl2 N32 C33 . . . 147.7(17) ? N31 N32 C33 . . . 107(2) ? N32 C33 C331 . . . 120(2) ? N32 C33 C34 . . . 112(2) ? C331 C33 C34 . . . 129(2) ? C33 C331 C332 . . . 122(2) ? C33 C331 C336 . . . 119(2) ? C33 C331 Tl3 . . 2 82.5(12) ? C332 C331 C336 . . . 119(2) ? C332 C331 Tl3 . . 2 107.3(13) ? C336 C331 Tl3 . . 2 81.1(13) ? C331 C332 C333 . . . 120(2) ? C331 C332 H332 . . . 120(2) ? C333 C332 H332 . . . 121(2) ? C332 C333 C334 . . . 121(2) ? C332 C333 H333 . . . 119(2) ? C334 C333 H333 . . . 119(3) ? C333 C334 C335 . . . 119(2) ? C333 C334 H334 . . . 120(2) ? C335 C334 H334 . . . 121(2) ? C334 C335 C336 . . . 121(2) ? C334 C335 H335 . . . 120(3) ? C336 C335 H335 . . . 120(3) ? C331 C336 C335 . . . 120(2) ? C331 C336 H336 . . . 119(2) ? C335 C336 H336 . . . 121(2) ? C33 C34 C35 . . . 108(2) ? C33 C34 H34 . . . 126(2) ? C35 C34 H34 . . . 126(2) ? Tl1 C35 N31 . . . 42.5(10) ? Tl1 C35 C34 . . . 131.5(14) ? Tl1 C35 C351 . . . 89.2(12) ? N31 C35 C34 . . . 106(2) ? N31 C35 C351 . . . 121(2) ? C34 C35 C351 . . . 133(2) ? C35 C351 C352 . . . 123(2) ? C35 C351 C356 . . . 121(2) ? C352 C351 C356 . . . 116(2) ? C351 C352 C353 . . . 124(2) ? C351 C352 H352 . . . 117(2) ? C353 C352 H352 . . . 119(2) ? C352 C353 C354 . . . 118(2) ? C352 C353 H353 . . . 120(2) ? C354 C353 H353 . . . 122(2) ? C353 C354 C355 . . . 122(2) ? C353 C354 H354 . . . 118(2) ? C355 C354 H354 . . . 119(2) ? C354 C355 C356 . . . 119(2) ? C354 C355 H355 . . . 122(2) ? C356 C355 H355 . . . 120(2) ? C351 C356 C355 . . . 121(2) ? C351 C356 H356 . . . 119(2) ? C355 C356 H356 . . . 120(2) ? Tl1 H152 C152 . . . 146.0(13) ? Tl3 H232 C232 . . . 108.8(14) ? Tl2 H252 C252 . . . 112.4(14) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Tl1 N12 3.503(19) . . ? Tl1 C15 3.77(2) . . ? Tl1 C151 4.10(2) . . ? Tl1 C152 3.61(2) . . ? Tl1 C23 3.87(2) . . ? Tl1 C235 4.12(3) . 3 ? Tl1 C25 3.69(2) . . ? Tl1 C254 4.16(3) . '1 655' ? Tl1 C255 4.02(3) . '1 655' ? Tl1 C335 4.02(2) . '2 545' ? Tl1 C351 3.73(2) . . ? Tl1 C352 3.62(2) . . ? Tl1 H235 3.6560(12) . 3 ? Tl1 H252 3.6568(11) . . ? Tl1 H255 3.7810(12) . '1 655' ? Tl1 H335 3.5366(11) . '2 545' ? Tl1 H352 3.2001(10) . . ? Tl2 C133 4.26(3) . . ? Tl2 C14 4.24(2) . . ? Tl2 C15 4.29(2) . . ? Tl2 C152 4.24(2) . '1 455' ? Tl2 C153 3.56(3) . '1 455' ? Tl2 C155 3.80(3) . '1 455' ? Tl2 N22 3.705(19) . . ? Tl2 C25 3.54(2) . . ? Tl2 C251 3.68(2) . . ? Tl2 C253 4.20(3) . . ? Tl2 C33 3.86(2) . . ? Tl2 C332 4.10(2) . . ? Tl2 C335 4.05(2) . '2 445' ? Tl2 H132 3.0873(11) . . ? Tl2 H153 3.6915(10) . '1 455' ? Tl2 H154 3.4920(11) . '1 455' ? Tl2 H332 3.3851(11) . . ? Tl2 H335 3.6329(10) . '2 445' ? Tl3 C13 3.59(2) . . ? Tl3 C131 4.27(2) . . ? Tl3 C132 4.00(2) . . ? Tl3 C15 4.12(2) . . ? Tl3 C151 3.59(2) . '2 545' ? Tl3 C156 3.60(2) . '2 545' ? Tl3 N21 3.644(18) . . ? Tl3 C231 3.65(2) . . ? Tl3 C33 3.59(2) . '2 545' ? Tl3 C332 4.09(2) . '2 545' ? Tl3 C335 4.17(3) . '2 545' ? Tl3 C336 3.53(2) . '2 545' ? Tl3 C34 3.52(2) . '2 545' ? Tl3 H132 3.2233(11) . . ? Tl3 H154 3.7603(12) . '2 545' ? Tl3 H336 3.5874(11) . '2 545' ? Tl3 H34 3.1935(11) . '2 545' ? N11 C13 2.17(3) . . ? N11 C14 2.20(3) . . ? N11 C151 2.46(3) . . ? N11 C152 2.99(3) . . ? N12 C131 2.44(3) . . ? N12 C132 2.88(3) . . ? N12 C14 2.24(3) . . ? N12 C15 2.21(3) . . ? C13 C132 2.52(3) . . ? C13 C136 2.53(3) . . ? C13 C15 2.17(3) . . ? C13 H14 2.14(2) . . ? C131 C133 2.44(3) . . ? C131 C134 2.84(3) . . ? C131 C135 2.42(4) . . ? C131 C14 2.59(3) . . ? C131 H132 2.12(2) . . ? C131 H136 2.05(2) . . ? C132 C134 2.46(4) . . ? C132 C135 2.78(4) . . ? C132 C136 2.42(3) . . ? C132 H133 2.06(2) . . ? C133 C135 2.32(4) . . ? C133 C136 2.72(3) . . ? C133 H132 2.13(3) . . ? C133 H134 2.03(3) . . ? C134 C136 2.40(3) . . ? C134 H133 2.01(2) . . ? C134 H135 2.01(2) . . ? C135 H134 2.05(3) . . ? C135 H136 2.04(3) . . ? C136 H135 2.04(2) . . ? C14 C151 2.53(3) . . ? C15 C152 2.50(3) . . ? C15 C156 2.47(3) . . ? C15 H14 2.08(2) . . ? C151 C153 2.43(3) . . ? C151 C154 2.81(3) . . ? C151 C155 2.45(3) . . ? C151 H152 2.02(2) . . ? C151 H156 2.03(2) . . ? C152 C154 2.42(3) . . ? C152 C155 2.75(3) . . ? C152 C156 2.33(3) . . ? C152 H153 2.11(2) . . ? C153 C155 2.34(4) . . ? C153 C156 2.72(4) . . ? C153 H152 2.10(2) . . ? C153 H154 2.03(2) . . ? C154 C156 2.38(3) . . ? C154 H153 2.03(2) . . ? C154 H155 2.01(2) . . ? C155 H154 2.01(3) . . ? C155 H156 2.07(3) . . ? C156 H155 2.08(2) . . ? N21 C23 2.20(3) . . ? N21 C24 2.20(3) . . ? N21 C251 2.48(3) . . ? N21 C252 2.96(3) . . ? N22 C231 2.44(3) . . ? N22 C232 2.95(3) . . ? N22 C24 2.20(3) . . ? N22 C25 2.21(3) . . ? C23 C232 2.51(3) . . ? C23 C236 2.49(3) . . ? C23 C25 2.19(3) . . ? C23 H24 2.12(2) . . ? C231 C233 2.47(3) . . ? C231 C234 2.80(3) . . ? C231 C235 2.41(3) . . ? C231 C24 2.57(3) . . ? C231 H232 2.08(2) . . ? C231 H236 2.02(2) . . ? C232 C234 2.42(3) . . ? C232 C235 2.77(3) . . ? C232 C236 2.39(3) . . ? C232 H233 2.10(2) . . ? C233 C235 2.37(3) . . ? C233 C236 2.77(3) . . ? C233 H232 2.11(3) . . ? C233 H234 2.03(3) . . ? C234 C236 2.39(3) . . ? C234 H233 2.04(2) . . ? C234 H235 2.02(2) . . ? C235 H234 2.01(3) . . ? C235 H236 2.05(3) . . ? C236 H235 2.06(2) . . ? C24 C251 2.57(3) . . ? C25 C252 2.52(3) . . ? C25 C256 2.50(3) . . ? C25 H24 2.09(2) . . ? C251 C253 2.42(3) . . ? C251 C254 2.78(3) . . ? C251 C255 2.37(3) . . ? C251 H252 2.03(2) . . ? C251 H256 2.04(2) . . ? C252 C254 2.36(3) . . ? C252 C255 2.70(3) . . ? C252 C256 2.34(3) . . ? C252 H253 2.07(2) . . ? C253 C255 2.36(3) . . ? C253 C256 2.74(3) . . ? C253 H252 2.05(2) . . ? C253 H254 2.03(2) . . ? C254 C256 2.37(3) . . ? C254 H253 2.02(3) . . ? C254 H255 2.04(3) . . ? C255 H254 2.07(2) . . ? C255 H256 2.00(2) . . ? C256 H255 2.01(2) . . ? N31 C33 2.16(3) . . ? N31 C34 2.21(3) . . ? N31 C351 2.47(3) . . ? N31 C352 2.97(3) . . ? N32 C331 2.47(3) . . ? N32 C332 2.96(3) . . ? N32 C34 2.18(3) . . ? N32 C35 2.22(3) . . ? C33 C332 2.57(4) . . ? C33 C336 2.57(4) . . ? C33 C35 2.17(4) . . ? C33 H34 2.05(3) . . ? C331 C333 2.34(4) . . ? C331 C334 2.77(4) . . ? C331 C335 2.43(4) . . ? C331 C34 2.59(3) . . ? C331 H332 2.05(2) . . ? C331 H336 2.09(2) . . ? C332 C334 2.43(3) . . ? C332 C335 2.80(3) . . ? C332 C336 2.43(3) . . ? C332 H333 1.98(2) . . ? C333 C335 2.41(4) . . ? C333 C336 2.74(3) . . ? C333 H332 2.00(3) . . ? C333 H334 2.12(3) . . ? C334 C336 2.35(4) . . ? C334 H333 2.11(3) . . ? C334 H335 1.99(3) . . ? C335 H334 2.01(3) . . ? C335 H336 2.04(3) . . ? C336 H335 2.02(2) . . ? C34 C351 2.58(3) . . ? C35 C352 2.50(3) . . ? C35 C356 2.47(3) . . ? C35 H34 2.10(2) . . ? C351 C353 2.41(3) . . ? C351 C354 2.75(4) . . ? C351 C355 2.41(3) . . ? C351 H352 2.03(2) . . ? C351 H356 2.05(2) . . ? C352 C354 2.30(4) . . ? C352 C355 2.71(3) . . ? C352 C356 2.35(3) . . ? C352 H353 2.01(3) . . ? C353 C355 2.38(3) . . ? C353 C356 2.75(3) . . ? C353 H352 1.99(2) . . ? C353 H354 2.02(2) . . ? C354 C356 2.36(3) . . ? C354 H353 2.04(2) . . ? C354 H355 2.05(2) . . ? C355 H354 2.04(2) . . ? C355 H356 2.04(3) . . ? C356 H355 2.04(2) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2352 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min -30 _reflns_limit_l_max 30 _reflns_number_observed ? _reflns_d_resolution_high .845 _reflns_d_resolution_low 13.28 _diffrn_reflns_av_sigmaI/netI .167 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .125 _refine_ls_wR_factor_all .076 _refine_ls_goodness_of_fit_all 1.443 _refine_ls_shift/su_mean .001 #===END data_ewantl _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(3,5-diphenylpyrazolato)thallium(I)].1,2-dimethoxyethane ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H54 N8 O2 Tl4' _chemical_formula_weight 1784.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Tl' 'Tl' -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p_1_21/n_1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.367(2) _cell_length_b 17.566(4) _cell_length_c 28.465(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.37(3) _cell_angle_gamma 90.00 _cell_volume 5674(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3336 _exptl_absorpt_coefficient_mu 11.378 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _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 'Enraf Nonius CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12968 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 28.31 _reflns_number_total 12968 _reflns_number_gt 9643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski and Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski and Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Siemans, 1993)' _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 w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+74.3534P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12968 _refine_ls_number_parameters 694 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1439 _refine_ls_wR_factor_gt 0.1328 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tl1 Tl 0.40188(3) 0.08338(2) 0.405284(14) 0.02087(10) Uani 1 d . . . Tl2 Tl 0.39669(3) 0.24687(2) 0.278491(14) 0.02130(10) Uani 1 d . . . Tl3 Tl 0.05359(3) 0.16759(2) 0.332843(14) 0.02010(10) Uani 1 d . . . Tl4 Tl 0.31218(3) 0.00542(2) 0.269167(15) 0.02232(11) Uani 1 d . . . N11 N 0.5161(7) 0.0655(5) 0.3252(3) 0.0207(18) Uani 1 d . . . N12 N 0.4961(8) 0.1063(5) 0.2851(3) 0.0227(19) Uani 1 d . . . N21 N 0.2140(8) 0.1263(5) 0.2288(3) 0.0226(19) Uani 1 d . . . N22 N 0.1814(7) 0.1874(5) 0.2575(3) 0.0188(18) Uani 1 d . . . N31 N 0.2428(8) 0.2121(5) 0.3807(3) 0.0207(19) Uani 1 d . . . N32 N 0.3558(7) 0.2262(5) 0.3652(3) 0.0177(17) Uani 1 d . . . N41 N 0.2063(8) 0.0165(5) 0.3734(3) 0.0204(19) Uani 1 d . . . N42 N 0.1323(8) 0.0321(5) 0.3343(3) 0.0199(18) Uani 1 d . . . C11 C 0.6319(9) 0.0476(6) 0.3302(4) 0.018(2) Uani 1 d . . . C12 C 0.6901(9) 0.0800(6) 0.2922(4) 0.023(2) Uani 1 d . . . H12 H 0.7717 0.0778 0.2867 0.027 Uiso 1 calc R . . C13 C 0.6011(9) 0.1158(6) 0.2648(4) 0.020(2) Uani 1 d . . . C111 C 0.6802(9) -0.0014(6) 0.3682(4) 0.024(2) Uani 1 d . . . C112 C 0.6081(11) -0.0555(6) 0.3895(4) 0.027(2) Uani 1 d . . . H112 H 0.5270 -0.0594 0.3797 0.032 Uiso 1 calc R . . C113 C 0.6546(12) -0.1020(7) 0.4239(4) 0.033(3) Uani 1 d . . . H113 H 0.6051 -0.1377 0.4383 0.040 Uiso 1 calc R . . C114 C 0.7742(12) -0.0982(7) 0.4386(4) 0.033(3) Uani 1 d . . . H114 H 0.8056 -0.1300 0.4632 0.040 Uiso 1 calc R . . C115 C 0.8447(12) -0.0482(8) 0.4170(5) 0.037(3) Uani 1 d . . . H115 H 0.9265 -0.0470 0.4259 0.044 Uiso 1 calc R . . C116 C 0.7999(10) 0.0010(6) 0.3821(5) 0.030(3) Uani 1 d . . . H116 H 0.8505 0.0360 0.3678 0.036 Uiso 1 calc R . . C131 C 0.6084(9) 0.1560(6) 0.2200(4) 0.022(2) Uani 1 d . . . C132 C 0.5089(10) 0.1582(6) 0.1883(4) 0.026(2) Uani 1 d . . . H132 H 0.4391 0.1316 0.1952 0.031 Uiso 1 calc R . . C133 C 0.5135(11) 0.1999(6) 0.1467(4) 0.028(3) Uani 1 d . . . H133 H 0.4464 0.2007 0.1252 0.034 Uiso 1 calc R . . C134 C 0.6127(14) 0.2399(7) 0.1360(4) 0.040(3) Uani 1 d . . . H134 H 0.6143 0.2681 0.1076 0.048 Uiso 1 calc R . . C135 C 0.7114(11) 0.2382(7) 0.1681(4) 0.034(3) Uani 1 d . . . H135 H 0.7811 0.2646 0.1611 0.041 Uiso 1 calc R . . C136 C 0.7076(11) 0.1975(7) 0.2104(4) 0.031(3) Uani 1 d . . . H136 H 0.7734 0.1984 0.2326 0.038 Uiso 1 calc R . . C21 C 0.1719(10) 0.1441(6) 0.1854(4) 0.024(2) Uani 1 d . . . C22 C 0.1125(10) 0.2133(6) 0.1843(4) 0.025(2) Uani 1 d . . . H22 H 0.0736 0.2369 0.1577 0.030 Uiso 1 calc R . . C23 C 0.1214(9) 0.2405(6) 0.2296(4) 0.021(2) Uani 1 d . . . C211 C 0.1900(10) 0.0907(6) 0.1450(4) 0.027(2) Uani 1 d . . . C212 C 0.2160(16) 0.1196(8) 0.1022(5) 0.053(4) Uani 1 d . . . H212 H 0.2236 0.1731 0.0983 0.063 Uiso 1 calc R . . C213 C 0.2315(17) 0.0713(9) 0.0644(5) 0.060(5) Uani 1 d . . . H213 H 0.2493 0.0918 0.0348 0.073 Uiso 1 calc R . . C214 C 0.2207(15) -0.0079(8) 0.0699(5) 0.048(4) Uani 1 d . . . H214 H 0.2349 -0.0416 0.0448 0.058 Uiso 1 calc R . . C215 C 0.1885(11) -0.0355(8) 0.1133(4) 0.035(3) Uani 1 d . . . H215 H 0.1751 -0.0885 0.1169 0.042 Uiso 1 calc R . . C216 C 0.1760(10) 0.0116(7) 0.1503(4) 0.029(3) Uani 1 d . . . H216 H 0.1577 -0.0087 0.1800 0.035 Uiso 1 calc R . . C231 C 0.0719(8) 0.3082(6) 0.2514(4) 0.017(2) Uani 1 d . . . C232 C 0.1121(9) 0.3340(6) 0.2950(4) 0.022(2) Uani 1 d . . . H232 H 0.1766 0.3090 0.3112 0.027 Uiso 1 calc R . . C233 C 0.0594(10) 0.3966(6) 0.3160(4) 0.027(2) Uani 1 d . . . H233 H 0.0867 0.4135 0.3464 0.032 Uiso 1 calc R . . C234 C -0.0357(10) 0.4345(6) 0.2909(5) 0.033(3) Uani 1 d . . . H234 H -0.0730 0.4767 0.3046 0.040 Uiso 1 calc R . . C235 C -0.0729(10) 0.4096(6) 0.2469(5) 0.031(3) Uani 1 d . . . H235 H -0.1349 0.4355 0.2298 0.037 Uiso 1 calc R . . C236 C -0.0205(9) 0.3468(6) 0.2272(4) 0.024(2) Uani 1 d . . . H236 H -0.0479 0.3298 0.1968 0.029 Uiso 1 calc R . . C31 C 0.2380(9) 0.2412(6) 0.4240(4) 0.020(2) Uani 1 d . . . C32 C 0.3456(9) 0.2769(6) 0.4377(4) 0.021(2) Uani 1 d . . . H32 H 0.3650 0.3030 0.4663 0.025 Uiso 1 calc R . . C33 C 0.4166(9) 0.2659(6) 0.4008(4) 0.021(2) Uani 1 d . . . C311 C 0.1348(10) 0.2311(6) 0.4516(4) 0.025(2) Uani 1 d . . . C312 C 0.0708(10) 0.1643(6) 0.4491(4) 0.026(2) Uani 1 d . . . H312 H 0.0943 0.1242 0.4293 0.031 Uiso 1 calc R . . C313 C -0.0270(11) 0.1553(8) 0.4752(5) 0.036(3) Uani 1 d . . . H313 H -0.0709 0.1093 0.4727 0.043 Uiso 1 calc R . . C314 C -0.0617(12) 0.2115(9) 0.5045(5) 0.042(3) Uani 1 d . . . H314 H -0.1287 0.2046 0.5225 0.051 Uiso 1 calc R . . C315 C 0.0038(12) 0.2801(8) 0.5077(4) 0.037(3) Uani 1 d . . . H315 H -0.0188 0.3197 0.5281 0.045 Uiso 1 calc R . . C316 C 0.1004(10) 0.2891(7) 0.4812(4) 0.027(2) Uani 1 d . . . H316 H 0.1439 0.3353 0.4831 0.032 Uiso 1 calc R . . C331 C 0.5425(9) 0.2829(6) 0.3975(4) 0.021(2) Uani 1 d . . . C332 C 0.6133(9) 0.2405(6) 0.3688(4) 0.024(2) Uani 1 d . . . H332 H 0.5783 0.2029 0.3485 0.028 Uiso 1 calc R . . C333 C 0.7363(10) 0.2526(7) 0.3695(5) 0.032(3) Uani 1 d . . . H333 H 0.7837 0.2233 0.3499 0.039 Uiso 1 calc R . . C334 C 0.7872(10) 0.3077(7) 0.3991(4) 0.031(3) Uani 1 d . . . H334 H 0.8698 0.3161 0.3999 0.037 Uiso 1 calc R . . C335 C 0.7174(11) 0.3506(7) 0.4276(5) 0.037(3) Uani 1 d . . . H335 H 0.7526 0.3886 0.4476 0.044 Uiso 1 calc R . . C336 C 0.5973(10) 0.3383(6) 0.4272(4) 0.023(2) Uani 1 d . . . H336 H 0.5509 0.3677 0.4472 0.028 Uiso 1 calc R . . C41 C 0.1973(9) -0.0588(6) 0.3828(4) 0.020(2) Uani 1 d . . . C42 C 0.1184(9) -0.0926(7) 0.3501(4) 0.024(2) Uani 1 d . . . H42 H 0.0963 -0.1447 0.3482 0.028 Uiso 1 calc R . . C43 C 0.0784(9) -0.0336(6) 0.3206(4) 0.021(2) Uani 1 d . . . C411 C 0.2626(9) -0.0919(6) 0.4235(4) 0.020(2) Uani 1 d . . . C412 C 0.2725(10) -0.0551(6) 0.4671(4) 0.022(2) Uani 1 d . . . H412 H 0.2386 -0.0060 0.4699 0.026 Uiso 1 calc R . . C413 C 0.3302(11) -0.0879(7) 0.5062(4) 0.032(3) Uani 1 d . . . H413 H 0.3352 -0.0621 0.5356 0.038 Uiso 1 calc R . . C414 C 0.3807(11) -0.1596(7) 0.5017(4) 0.033(3) Uani 1 d . . . H414 H 0.4231 -0.1822 0.5279 0.040 Uiso 1 calc R . . C415 C 0.3694(11) -0.1977(7) 0.4595(5) 0.034(3) Uani 1 d . . . H415 H 0.4001 -0.2478 0.4574 0.041 Uiso 1 calc R . . C416 C 0.3137(9) -0.1643(6) 0.4197(4) 0.025(2) Uani 1 d . . . H416 H 0.3103 -0.1902 0.3903 0.031 Uiso 1 calc R . . C431 C -0.0055(9) -0.0388(6) 0.2791(4) 0.020(2) Uani 1 d . . . C432 C -0.0199(9) 0.0199(7) 0.2470(4) 0.025(2) Uani 1 d . . . H432 H 0.0208 0.0665 0.2527 0.030 Uiso 1 calc R . . C433 C -0.0941(10) 0.0115(7) 0.2061(4) 0.033(3) Uani 1 d . . . H433 H -0.1028 0.0519 0.1840 0.040 Uiso 1 calc R . . C434 C -0.1551(11) -0.0570(8) 0.1982(5) 0.034(3) Uani 1 d . . . H434 H -0.2033 -0.0638 0.1701 0.041 Uiso 1 calc R . . C435 C -0.1457(10) -0.1127(7) 0.2300(4) 0.031(3) Uani 1 d . . . H435 H -0.1894 -0.1584 0.2251 0.037 Uiso 1 calc R . . C436 C -0.0704(10) -0.1039(6) 0.2714(4) 0.027(2) Uani 1 d . . . H436 H -0.0650 -0.1436 0.2940 0.032 Uiso 1 calc R . . O1 O 0.8644(9) 0.1169(6) 0.0354(3) 0.046(2) Uani 1 d . . . O2 O 0.6591(19) 0.0292(13) 0.0468(8) 0.042(5) Uiso 0.50 d P A 1 O2' O 0.628(2) 0.0521(15) 0.0558(9) 0.056(6) Uiso 0.50 d P A 2 C61 C 0.865(3) 0.1926(17) 0.0615(11) 0.047(7) Uiso 0.50 d P B 1 H61A H 0.8556 0.2344 0.0387 0.070 Uiso 0.50 calc PR B 1 H61B H 0.9398 0.1986 0.0800 0.070 Uiso 0.50 calc PR B 1 H61C H 0.7998 0.1937 0.0826 0.070 Uiso 0.50 calc PR B 1 C62 C 0.869(3) 0.0577(18) 0.0621(11) 0.049(7) Uiso 0.50 d P A 1 H62A H 0.9301 0.0656 0.0879 0.058 Uiso 0.50 calc PR A 1 H62B H 0.8927 0.0131 0.0436 0.058 Uiso 0.50 calc PR A 1 C63 C 0.751(3) 0.0412(18) 0.0830(11) 0.040(7) Uiso 0.50 d P A 1 H63A H 0.7590 -0.0047 0.1032 0.048 Uiso 0.50 calc PR A 1 H63B H 0.7298 0.0845 0.1031 0.048 Uiso 0.50 calc PR A 1 C61' C 0.947(3) 0.0510(17) 0.0432(11) 0.045(7) Uiso 0.50 d P B 2 H61D H 0.9907 0.0430 0.0149 0.068 Uiso 0.50 calc PR B 2 H61E H 0.9022 0.0051 0.0498 0.068 Uiso 0.50 calc PR B 2 H61F H 1.0029 0.0620 0.0699 0.068 Uiso 0.50 calc PR B 2 C62' C 0.798(3) 0.1330(18) 0.0741(11) 0.050(7) Uiso 0.50 d P A 2 H62C H 0.7484 0.1783 0.0665 0.061 Uiso 0.50 calc PR A 2 H62D H 0.8525 0.1466 0.1012 0.061 Uiso 0.50 calc PR A 2 C63' C 0.717(3) 0.0688(17) 0.0895(11) 0.039(6) Uiso 0.50 d P A 2 H63C H 0.7653 0.0225 0.0960 0.047 Uiso 0.50 calc PR A 2 H63D H 0.6818 0.0837 0.1191 0.047 Uiso 0.50 calc PR A 2 C64 C 0.5415(17) 0.0091(11) 0.0678(7) 0.070(5) Uiso 1 d . . . H64A H 0.4806 0.0022 0.0423 0.104 Uiso 1 calc R C 1 H64B H 0.5184 0.0504 0.0885 0.104 Uiso 1 calc R C 1 H64C H 0.5505 -0.0381 0.0860 0.104 Uiso 1 calc R C 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl1 0.0218(2) 0.0181(2) 0.0225(2) 0.00080(15) -0.00077(15) -0.00028(15) Tl2 0.0213(2) 0.0195(2) 0.0234(2) 0.00070(15) 0.00359(15) -0.00067(15) Tl3 0.01761(19) 0.0188(2) 0.0240(2) 0.00196(15) 0.00201(15) 0.00171(14) Tl4 0.0202(2) 0.0165(2) 0.0305(2) -0.00178(16) 0.00368(16) 0.00052(14) N11 0.016(4) 0.019(5) 0.026(5) 0.003(4) 0.000(4) 0.002(3) N12 0.023(5) 0.025(5) 0.020(5) 0.002(4) 0.000(4) -0.006(4) N21 0.017(4) 0.021(5) 0.029(5) -0.011(4) 0.002(4) 0.001(3) N22 0.016(4) 0.011(4) 0.029(5) -0.005(3) 0.002(4) -0.005(3) N31 0.020(4) 0.013(4) 0.029(5) 0.003(3) 0.001(4) 0.001(3) N32 0.016(4) 0.014(4) 0.024(5) -0.003(3) 0.003(3) 0.004(3) N41 0.029(5) 0.015(4) 0.017(4) 0.001(3) -0.003(4) 0.003(3) N42 0.021(4) 0.013(4) 0.025(5) -0.004(3) 0.000(4) 0.000(3) C11 0.018(5) 0.019(5) 0.018(5) -0.005(4) 0.007(4) -0.001(4) C12 0.020(5) 0.020(6) 0.028(6) -0.008(4) 0.007(4) -0.001(4) C13 0.020(5) 0.017(5) 0.024(6) -0.008(4) 0.003(4) 0.004(4) C111 0.023(5) 0.020(6) 0.030(6) -0.002(4) -0.002(4) 0.002(4) C112 0.035(6) 0.019(6) 0.028(6) 0.001(4) 0.011(5) 0.003(4) C113 0.050(8) 0.019(6) 0.032(7) -0.003(5) 0.008(6) -0.004(5) C114 0.046(8) 0.030(7) 0.023(6) 0.001(5) 0.002(5) 0.016(5) C115 0.036(7) 0.046(8) 0.029(7) -0.002(6) -0.001(6) 0.012(6) C116 0.026(6) 0.022(6) 0.041(7) -0.002(5) 0.000(5) 0.004(4) C131 0.020(5) 0.020(6) 0.025(6) -0.005(4) 0.005(4) 0.005(4) C132 0.029(6) 0.025(6) 0.025(6) -0.004(5) 0.005(5) -0.006(4) C133 0.041(7) 0.026(6) 0.019(6) 0.001(4) 0.003(5) 0.000(5) C134 0.077(10) 0.028(7) 0.017(6) -0.001(5) 0.011(6) 0.000(6) C135 0.037(7) 0.046(8) 0.022(6) -0.007(5) 0.016(5) -0.009(6) C136 0.030(6) 0.032(7) 0.033(7) 0.001(5) 0.006(5) -0.013(5) C21 0.025(6) 0.018(5) 0.030(6) -0.004(4) -0.004(5) -0.007(4) C22 0.026(6) 0.023(6) 0.026(6) 0.006(4) 0.001(5) 0.002(4) C23 0.020(5) 0.019(5) 0.024(5) 0.001(4) 0.002(4) -0.006(4) C211 0.035(6) 0.025(6) 0.019(5) -0.008(4) -0.007(5) 0.007(5) C212 0.097(13) 0.034(8) 0.026(7) -0.011(6) -0.005(8) 0.009(8) C213 0.099(14) 0.057(10) 0.024(7) 0.001(7) -0.005(8) -0.004(9) C214 0.076(11) 0.037(8) 0.030(7) -0.018(6) -0.007(7) 0.018(7) C215 0.040(7) 0.034(7) 0.029(7) -0.010(5) 0.001(6) -0.002(5) C216 0.032(6) 0.029(6) 0.025(6) -0.007(5) -0.001(5) -0.003(5) C231 0.014(5) 0.014(5) 0.024(5) 0.006(4) 0.004(4) 0.001(4) C232 0.025(5) 0.012(5) 0.030(6) 0.003(4) 0.007(4) -0.002(4) C233 0.022(6) 0.022(6) 0.037(7) -0.003(5) 0.012(5) -0.010(4) C234 0.024(6) 0.014(6) 0.063(9) 0.008(5) 0.014(6) 0.004(4) C235 0.027(6) 0.018(6) 0.048(8) 0.007(5) 0.004(5) 0.004(4) C236 0.015(5) 0.027(6) 0.031(6) 0.004(5) 0.008(4) -0.001(4) C31 0.029(6) 0.012(5) 0.019(5) 0.005(4) 0.002(4) 0.000(4) C32 0.020(5) 0.017(5) 0.026(6) -0.007(4) 0.006(4) -0.010(4) C33 0.020(5) 0.021(6) 0.022(5) 0.004(4) 0.000(4) 0.001(4) C311 0.031(6) 0.028(6) 0.015(5) 0.005(4) 0.001(4) 0.007(5) C312 0.027(6) 0.027(6) 0.022(6) 0.009(4) -0.001(4) -0.004(5) C313 0.029(6) 0.043(8) 0.035(7) 0.012(6) -0.004(5) -0.015(5) C314 0.036(7) 0.065(10) 0.028(7) 0.003(6) 0.007(6) -0.012(6) C315 0.040(7) 0.049(8) 0.024(7) -0.007(5) 0.012(6) 0.002(6) C316 0.027(6) 0.030(6) 0.024(6) -0.003(5) 0.003(5) 0.003(5) C331 0.025(6) 0.017(5) 0.020(5) 0.005(4) -0.006(4) 0.002(4) C332 0.018(5) 0.028(6) 0.025(6) -0.003(4) 0.002(4) 0.002(4) C333 0.014(5) 0.037(7) 0.046(8) -0.001(6) 0.001(5) 0.002(5) C334 0.012(5) 0.042(7) 0.038(7) -0.001(5) -0.002(5) -0.004(5) C335 0.033(7) 0.036(7) 0.040(8) -0.004(6) -0.005(6) -0.014(5) C336 0.028(6) 0.019(6) 0.024(6) 0.000(4) 0.012(4) -0.005(4) C41 0.020(5) 0.015(5) 0.024(6) 0.002(4) 0.003(4) -0.001(4) C42 0.022(5) 0.031(6) 0.018(5) -0.003(4) 0.001(4) -0.001(4) C43 0.015(5) 0.022(6) 0.026(6) -0.003(4) 0.003(4) 0.006(4) C411 0.013(5) 0.023(6) 0.024(5) 0.007(4) 0.005(4) 0.000(4) C412 0.031(6) 0.016(5) 0.019(5) 0.000(4) -0.002(4) -0.002(4) C413 0.035(7) 0.033(7) 0.028(6) 0.001(5) -0.003(5) -0.008(5) C414 0.032(7) 0.032(7) 0.033(7) 0.009(5) -0.014(5) -0.002(5) C415 0.033(7) 0.014(6) 0.053(8) 0.003(5) -0.006(6) 0.005(5) C416 0.020(5) 0.014(5) 0.043(7) -0.001(5) 0.005(5) -0.003(4) C431 0.018(5) 0.026(6) 0.017(5) -0.003(4) 0.004(4) 0.002(4) C432 0.015(5) 0.032(6) 0.029(6) -0.004(5) 0.006(4) -0.003(4) C433 0.026(6) 0.042(7) 0.031(7) -0.006(5) 0.004(5) -0.002(5) C434 0.025(6) 0.047(8) 0.030(7) -0.004(6) -0.006(5) 0.002(5) C435 0.024(6) 0.031(7) 0.037(7) -0.016(5) 0.001(5) -0.003(5) C436 0.023(6) 0.021(6) 0.036(7) -0.007(5) 0.000(5) -0.001(4) O1 0.056(6) 0.046(6) 0.037(6) 0.000(4) 0.007(5) 0.016(5) _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 Tl1 N41 2.628(9) . ? Tl1 N11 2.706(9) . ? Tl1 N32 2.794(8) . ? Tl1 N31 2.953(8) . ? Tl2 N32 2.563(9) . ? Tl2 N22 2.696(8) . ? Tl2 N12 2.718(9) . ? Tl3 N42 2.542(8) . ? Tl3 N31 2.597(9) . ? Tl3 N22 2.682(9) . ? Tl4 N21 2.632(9) . ? Tl4 N12 2.757(9) . ? Tl4 N42 2.878(9) . ? Tl4 N11 2.932(9) . ? N11 C11 1.353(13) . ? N11 N12 1.356(12) . ? N12 C13 1.368(14) . ? N21 C21 1.335(14) . ? N21 N22 1.412(12) . ? N22 C23 1.379(13) . ? N31 C31 1.339(14) . ? N31 N32 1.405(12) . ? N32 C33 1.383(13) . ? N41 C41 1.356(13) . ? N41 N42 1.383(12) . ? N42 C43 1.353(14) . ? C11 C12 1.420(15) . ? C11 C111 1.464(15) . ? C12 C13 1.391(15) . ? C13 C131 1.462(15) . ? C111 C116 1.395(16) . ? C111 C112 1.415(15) . ? C112 C113 1.358(17) . ? C113 C114 1.400(18) . ? C114 C115 1.360(19) . ? C115 C116 1.390(17) . ? C131 C136 1.383(15) . ? C131 C132 1.405(15) . ? C132 C133 1.397(16) . ? C133 C134 1.378(18) . ? C134 C135 1.40(2) . ? C135 C136 1.404(17) . ? C21 C22 1.390(15) . ? C21 C211 1.508(15) . ? C22 C23 1.375(15) . ? C23 C231 1.467(14) . ? C211 C212 1.367(19) . ? C211 C216 1.407(17) . ? C212 C213 1.39(2) . ? C213 C214 1.41(2) . ? C214 C215 1.39(2) . ? C215 C216 1.355(16) . ? C231 C232 1.373(15) . ? C231 C236 1.398(14) . ? C232 C233 1.403(15) . ? C233 C234 1.425(17) . ? C234 C235 1.369(19) . ? C235 C236 1.388(16) . ? C31 C32 1.408(14) . ? C31 C311 1.460(15) . ? C32 C33 1.373(15) . ? C33 C331 1.470(15) . ? C311 C312 1.380(16) . ? C311 C316 1.393(15) . ? C312 C313 1.382(17) . ? C313 C314 1.36(2) . ? C314 C315 1.42(2) . ? C315 C316 1.378(17) . ? C331 C332 1.395(15) . ? C331 C336 1.410(15) . ? C332 C333 1.413(15) . ? C333 C334 1.386(17) . ? C334 C335 1.389(18) . ? C335 C336 1.382(16) . ? C41 C42 1.388(15) . ? C41 C411 1.458(14) . ? C42 C43 1.393(15) . ? C43 C431 1.477(15) . ? C411 C412 1.396(15) . ? C411 C416 1.406(15) . ? C412 C413 1.385(16) . ? C413 C414 1.392(18) . ? C414 C415 1.375(18) . ? C415 C416 1.395(17) . ? C431 C436 1.370(15) . ? C431 C432 1.380(16) . ? C432 C433 1.405(16) . ? C433 C434 1.400(18) . ? C434 C435 1.334(18) . ? C435 C436 1.423(16) . ? O1 C62 1.29(3) . ? O1 C62' 1.40(3) . ? O1 C61' 1.50(3) . ? O1 C61 1.52(3) . ? O2 C63 1.44(4) . ? O2 C64 1.54(3) . ? O2' C64 1.30(3) . ? O2' C63' 1.38(4) . ? C62 C63 1.53(4) . ? C62' C63' 1.53(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N41 Tl1 N11 95.5(3) . . ? N41 Tl1 N32 97.2(3) . . ? N11 Tl1 N32 81.3(3) . . ? N41 Tl1 N31 76.5(2) . . ? N11 Tl1 N31 101.9(3) . . ? N32 Tl1 N31 28.1(2) . . ? N32 Tl2 N22 86.8(3) . . ? N32 Tl2 N12 84.4(3) . . ? N22 Tl2 N12 91.8(3) . . ? N42 Tl3 N31 89.6(3) . . ? N42 Tl3 N22 85.8(3) . . ? N31 Tl3 N22 84.8(3) . . ? N21 Tl4 N12 81.5(3) . . ? N21 Tl4 N42 81.4(3) . . ? N12 Tl4 N42 110.5(3) . . ? N21 Tl4 N11 104.4(3) . . ? N12 Tl4 N11 27.4(2) . . ? N42 Tl4 N11 99.2(2) . . ? C11 N11 N12 108.9(8) . . ? C11 N11 Tl1 116.9(7) . . ? N12 N11 Tl1 125.7(6) . . ? C11 N11 Tl4 134.9(7) . . ? N12 N11 Tl4 69.1(5) . . ? Tl1 N11 Tl4 95.6(3) . . ? N11 N12 C13 108.3(9) . . ? N11 N12 Tl2 125.9(7) . . ? C13 N12 Tl2 103.2(6) . . ? N11 N12 Tl4 83.5(5) . . ? C13 N12 Tl4 133.0(7) . . ? Tl2 N12 Tl4 105.3(3) . . ? C21 N21 N22 105.4(8) . . ? C21 N21 Tl4 135.5(7) . . ? N22 N21 Tl4 118.6(6) . . ? C23 N22 N21 108.6(8) . . ? C23 N22 Tl3 106.0(6) . . ? N21 N22 Tl3 122.5(6) . . ? C23 N22 Tl2 106.0(6) . . ? N21 N22 Tl2 99.0(5) . . ? Tl3 N22 Tl2 113.6(3) . . ? C31 N31 N32 108.0(8) . . ? C31 N31 Tl3 121.4(7) . . ? N32 N31 Tl3 129.2(6) . . ? C31 N31 Tl1 97.6(6) . . ? N32 N31 Tl1 69.6(5) . . ? Tl3 N31 Tl1 111.8(3) . . ? C33 N32 N31 106.6(8) . . ? C33 N32 Tl2 121.6(7) . . ? N31 N32 Tl2 123.3(6) . . ? C33 N32 Tl1 94.5(6) . . ? N31 N32 Tl1 82.3(5) . . ? Tl2 N32 Tl1 118.7(3) . . ? C41 N41 N42 107.7(8) . . ? C41 N41 Tl1 116.1(7) . . ? N42 N41 Tl1 130.7(6) . . ? C43 N42 N41 107.9(8) . . ? C43 N42 Tl3 129.9(6) . . ? N41 N42 Tl3 113.3(6) . . ? C43 N42 Tl4 90.1(6) . . ? N41 N42 Tl4 93.7(6) . . ? Tl3 N42 Tl4 113.9(3) . . ? N11 C11 C12 108.8(9) . . ? N11 C11 C111 122.3(9) . . ? C12 C11 C111 128.9(10) . . ? C13 C12 C11 104.6(9) . . ? N12 C13 C12 109.3(10) . . ? N12 C13 C131 121.6(9) . . ? C12 C13 C131 129.1(10) . . ? C116 C111 C112 118.6(10) . . ? C116 C111 C11 120.6(10) . . ? C112 C111 C11 120.7(10) . . ? C113 C112 C111 120.2(12) . . ? C112 C113 C114 121.1(12) . . ? C115 C114 C113 118.9(11) . . ? C114 C115 C116 121.6(12) . . ? C115 C116 C111 119.6(12) . . ? C136 C131 C132 119.6(11) . . ? C136 C131 C13 121.0(10) . . ? C132 C131 C13 119.2(10) . . ? C133 C132 C131 119.4(11) . . ? C134 C133 C132 121.7(12) . . ? C133 C134 C135 118.6(11) . . ? C136 C135 C134 120.3(12) . . ? C131 C136 C135 120.3(12) . . ? N21 C21 C22 111.9(10) . . ? N21 C21 C211 120.2(10) . . ? C22 C21 C211 127.9(10) . . ? C23 C22 C21 105.9(10) . . ? C22 C23 N22 108.2(9) . . ? C22 C23 C231 132.0(10) . . ? N22 C23 C231 119.6(9) . . ? C212 C211 C216 119.7(11) . . ? C212 C211 C21 119.6(11) . . ? C216 C211 C21 120.6(11) . . ? C211 C212 C213 120.4(14) . . ? C212 C213 C214 120.0(15) . . ? C215 C214 C213 118.3(12) . . ? C216 C215 C214 121.4(12) . . ? C215 C216 C211 120.1(12) . . ? C232 C231 C236 119.1(10) . . ? C232 C231 C23 122.2(9) . . ? C236 C231 C23 118.7(10) . . ? C231 C232 C233 121.1(10) . . ? C232 C233 C234 118.9(11) . . ? C235 C234 C233 119.6(11) . . ? C234 C235 C236 120.5(11) . . ? C235 C236 C231 120.9(11) . . ? N31 C31 C32 110.1(9) . . ? N31 C31 C311 121.7(10) . . ? C32 C31 C311 128.2(10) . . ? C33 C32 C31 105.5(9) . . ? C32 C33 N32 109.9(9) . . ? C32 C33 C331 129.7(10) . . ? N32 C33 C331 120.1(9) . . ? C312 C311 C316 119.1(11) . . ? C312 C311 C31 120.9(10) . . ? C316 C311 C31 120.0(10) . . ? C311 C312 C313 120.5(12) . . ? C314 C313 C312 121.1(12) . . ? C313 C314 C315 119.0(12) . . ? C316 C315 C314 119.7(12) . . ? C315 C316 C311 120.6(11) . . ? C332 C331 C336 118.0(10) . . ? C332 C331 C33 121.8(10) . . ? C336 C331 C33 119.9(10) . . ? C331 C332 C333 121.0(11) . . ? C334 C333 C332 119.4(11) . . ? C333 C334 C335 120.1(10) . . ? C336 C335 C334 120.5(11) . . ? C335 C336 C331 120.9(10) . . ? N41 C41 C42 109.7(10) . . ? N41 C41 C411 120.3(9) . . ? C42 C41 C411 129.9(10) . . ? C41 C42 C43 105.2(10) . . ? N42 C43 C42 109.6(9) . . ? N42 C43 C431 122.9(9) . . ? C42 C43 C431 127.5(10) . . ? C412 C411 C416 118.4(10) . . ? C412 C411 C41 122.1(10) . . ? C416 C411 C41 119.5(10) . . ? C413 C412 C411 122.1(10) . . ? C412 C413 C414 118.7(11) . . ? C415 C414 C413 120.2(11) . . ? C414 C415 C416 121.3(11) . . ? C415 C416 C411 119.2(11) . . ? C436 C431 C432 118.4(10) . . ? C436 C431 C43 119.7(10) . . ? C432 C431 C43 121.9(10) . . ? C431 C432 C433 120.8(11) . . ? C434 C433 C432 119.3(12) . . ? C435 C434 C433 120.2(12) . . ? C434 C435 C436 120.1(11) . . ? C431 C436 C435 121.0(11) . . ? C62 O1 C62' 72.9(19) . . ? C62 O1 C61' 44.4(17) . . ? C62' O1 C61' 113.8(19) . . ? C62 O1 C61 115(2) . . ? C62' O1 C61 55.1(17) . . ? C61' O1 C61 128.2(18) . . ? C63 O2 C64 112(2) . . ? C64 O2' C63' 118(2) . . ? O1 C62 C63 112(3) . . ? O2 C63 C62 112(2) . . ? O1 C62' C63' 116(2) . . ? O2' C63' C62' 112(3) . . ? O2' C64 O2 22.5(13) . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 4.825 _refine_diff_density_min -2.911 _refine_diff_density_rms 0.304 #===END data_gbdtll # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C92 H72 Cl4 N12 O2 Tl8' _chemical_formula_moiety ? _chemical_formula_weight 3154.55 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 13.851(2) _cell_length_b 21.533(4) _cell_length_c 14.721(3) _cell_angle_alpha 90.00000 _cell_angle_beta 92.160(3) _cell_angle_gamma 90.00000 _cell_volume 4387.5(14) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 2.388 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5806 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 14.811 _exptl_crystal_description prism _exptl_crystal_size_max .5 _exptl_crystal_size_mid .39 _exptl_crystal_size_min .22 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .096 _exptl_absorpt_correction_T_max .432 _diffrn_reflns_number 50455 _reflns_number_total 11124 _reflns_Friedel_coverage 0 _reflns_number_gt 7654 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.23 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .082 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% ? #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .038 _refine_ls_wR_factor_ref .042 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_number_reflns 7654 _refine_ls_number_parameters 534 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .049 _refine_diff_density_min -1.714 _refine_diff_density_max 2.533 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 1768(109) _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 184 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 24 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 144 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Tl ? 0 16 -3.556 9.659 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 8 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Tl1 .55529(2) .040031(16) .59284(2) .02243(17) Uani ? ? 1.00000 ? ? Tl2 .40878(2) -.024038(15) .80914(2) .02182(17) Uani ? ? 1.00000 ? ? Tl3 .38131(2) .171195(15) .73201(2) .02192(17) Uani ? ? 1.00000 ? ? Tl4 .25246(3) .050784(17) .56326(3) .0289(2) Uani ? ? 1.00000 ? ? O0 .4068(4) .0995(3) .6028(4) .023(3) Uani ? ? 1.00000 ? ? N11 .5716(5) .0664(3) .7660(4) .018(3) Uani ? ? 1.00000 ? ? N12 .4949(5) .0904(3) .8131(4) .023(4) Uani ? ? 1.00000 ? ? C13 .5249(6) .0956(4) .9020(5) .021(4) Uani ? ? 1.00000 ? ? C131 .4596(6) .1191(4) .9699(5) .018(4) Uani ? ? 1.00000 ? ? C132 .3596(6) .1150(4) .9599(6) .022(4) Uani ? ? 1.00000 ? ? C133 .3012(6) .1376(4) 1.0266(6) .025(5) Uani ? ? 1.00000 ? ? C134 .3402(6) .1644(4) 1.1038(6) .026(5) Uani ? ? 1.00000 ? ? C135 .4389(7) .1698(4) 1.1159(6) .030(5) Uani ? ? 1.00000 ? ? C136 .4980(6) .1482(4) 1.0491(6) .024(5) Uani ? ? 1.00000 ? ? C14 .6192(6) .0735(4) .9132(6) .023(4) Uani ? ? 1.00000 ? ? C15 .6448(6) .0561(4) .8248(5) .018(4) Uani ? ? 1.00000 ? ? C151 .7383(6) .0312(4) .7968(6) .020(4) Uani ? ? 1.00000 ? ? C152 .7887(6) -.0112(4) .8524(6) .024(5) Uani ? ? 1.00000 ? ? C153 .8794(7) -.0341(4) .8297(6) .029(5) Uani ? ? 1.00000 ? ? C154 .9193(6) -.0150(4) .7515(6) .029(5) Uani ? ? 1.00000 ? ? C155 .8707(7) .0280(4) .6946(6) .031(5) Uani ? ? 1.00000 ? ? C156 .7808(6) .0506(4) .7183(6) .025(5) Uani ? ? 1.00000 ? ? N21 .4227(5) -.0616(3) .6335(5) .024(4) Uani ? ? 1.00000 ? ? N22 .3259(5) -.0552(3) .6125(5) .022(4) Uani ? ? 1.00000 ? ? C23 .2938(6) -.1085(4) .5745(5) .018(4) Uani ? ? 1.00000 ? ? C231 .1916(6) -.1170(4) .5425(5) .021(4) Uani ? ? 1.00000 ? ? C232 .1165(7) -.0828(4) .5792(6) .027(5) Uani ? ? 1.00000 ? ? C233 .0227(6) -.0897(5) .5456(6) .032(5) Uani ? ? 1.00000 ? ? C234 .0007(7) -.1324(5) .4785(7) .036(6) Uani ? ? 1.00000 ? ? C235 .0727(6) -.1677(4) .4426(7) .031(5) Uani ? ? 1.00000 ? ? C236 .1678(6) -.1600(4) .4744(6) .026(5) Uani ? ? 1.00000 ? ? C24 .3700(6) -.1512(4) .5695(5) .022(4) Uani ? ? 1.00000 ? ? C25 .4503(6) -.1197(4) .6076(5) .022(4) Uani ? ? 1.00000 ? ? C251 .5496(6) -.1402(4) .6163(5) .020(4) Uani ? ? 1.00000 ? ? C252 .6209(7) -.1076(4) .6681(5) .024(4) Uani ? ? 1.00000 ? ? C253 .7170(6) -.1241(4) .6705(6) .025(5) Uani ? ? 1.00000 ? ? C254 .7444(7) -.1756(5) .6244(7) .035(5) Uani ? ? 1.00000 ? ? C255 .6763(7) -.2117(4) .5773(6) .032(5) Uani ? ? 1.00000 ? ? C256 .5793(7) -.1932(4) .5722(6) .027(5) Uani ? ? 1.00000 ? ? N31 .2309(5) .0965(3) .7470(5) .024(4) Uani ? ? 1.00000 ? ? N32 .2451(5) .0358(3) .7744(5) .021(4) Uani ? ? 1.00000 ? ? C33 .1713(6) .0209(3) .8280(5) .017(4) Uani ? ? 1.00000 ? ? C331 .1649(6) -.0421(4) .8696(5) .019(4) Uani ? ? 1.00000 ? ? C332 .2012(6) -.0947(4) .8279(6) .025(5) Uani ? ? 1.00000 ? ? C333 .1979(7) -.1527(4) .8688(6) .030(5) Uani ? ? 1.00000 ? ? C334 .1603(7) -.1572(4) .9535(7) .037(6) Uani ? ? 1.00000 ? ? C335 .1217(7) -.1062(4) .9943(6) .032(5) Uani ? ? 1.00000 ? ? C336 .1232(6) -.0494(4) .9542(6) .022(4) Uani ? ? 1.00000 ? ? C34 .1112(6) .0718(4) .8378(6) .023(4) Uani ? ? 1.00000 ? ? C35 .1500(6) .1180(4) .7857(5) .019(4) Uani ? ? 1.00000 ? ? C351 .1128(6) .1812(4) .7678(7) .027(5) Uani ? ? 1.00000 ? ? C352 .1363(6) .2151(4) .6904(7) .030(5) Uani ? ? 1.00000 ? ? C353 .0976(6) .2743(4) .6748(8) .040(6) Uani ? ? 1.00000 ? ? C354 .0331(7) .2990(4) .7333(9) .050(7) Uani ? ? 1.00000 ? ? C355 .0073(7) .2664(4) .8090(8) .043(6) Uani ? ? 1.00000 ? ? C356 .0482(6) .2081(4) .8264(7) .033(5) Uani ? ? 1.00000 ? ? Cl1 .62130(17) .20834(12) .66119(16) .0368(13) Uani ? ? 1.00000 ? ? Cl2 .7716(2) .21813(15) .8044(2) .0572(18) Uani ? ? 1.00000 ? ? C0 .6478(7) .2166(5) .7796(6) .036(6) Uani ? ? 1.00000 ? ? H0 .41315 .11560 .55065 .02800 Uiso ? ? 1.00000 ? ? H132 .33075 .09678 .90521 .03000 Uiso ? ? 1.00000 ? ? H133 .23156 .13410 1.01934 .03300 Uiso ? ? 1.00000 ? ? H134 .29843 .17928 1.14941 .03400 Uiso ? ? 1.00000 ? ? H135 .46570 .18864 1.17030 .03700 Uiso ? ? 1.00000 ? ? H136 .56742 .15258 1.05713 .03100 Uiso ? ? 1.00000 ? ? H14 .65734 .07012 .96909 .02700 Uiso ? ? 1.00000 ? ? H152 .76002 -.02474 .90743 .03000 Uiso ? ? 1.00000 ? ? H153 .91377 -.06287 .86947 .03600 Uiso ? ? 1.00000 ? ? H154 .98085 -.03079 .73576 .03700 Uiso ? ? 1.00000 ? ? H155 .89946 .04132 .63943 .03900 Uiso ? ? 1.00000 ? ? H156 .74780 .08053 .67954 .03200 Uiso ? ? 1.00000 ? ? H232 .13062 -.05398 .62787 .03500 Uiso ? ? 1.00000 ? ? H233 -.02766 -.06447 .56997 .03800 Uiso ? ? 1.00000 ? ? H234 -.06598 -.13842 .45705 .04600 Uiso ? ? 1.00000 ? ? H235 .05850 -.19785 .39498 .03800 Uiso ? ? 1.00000 ? ? H236 .21814 -.18470 .44897 .03200 Uiso ? ? 1.00000 ? ? H24 .36816 -.19288 .54539 .02700 Uiso ? ? 1.00000 ? ? H252 .60102 -.07246 .70295 .03000 Uiso ? ? 1.00000 ? ? H253 .76406 -.09939 .70482 .03100 Uiso ? ? 1.00000 ? ? H254 .81254 -.18614 .62376 .04500 Uiso ? ? 1.00000 ? ? H255 .69518 -.25019 .54861 .04200 Uiso ? ? 1.00000 ? ? H256 .53221 -.21754 .53739 .03300 Uiso ? ? 1.00000 ? ? H332 .22956 -.09066 .76913 .03100 Uiso ? ? 1.00000 ? ? H333 .22112 -.18860 .83781 .03700 Uiso ? ? 1.00000 ? ? H334 .16245 -.19695 .98509 .04600 Uiso ? ? 1.00000 ? ? H335 .09311 -.11053 1.05335 .04100 Uiso ? ? 1.00000 ? ? H336 .09654 -.01365 .98403 .02800 Uiso ? ? 1.00000 ? ? H34 .05461 .07434 .87371 .02800 Uiso ? ? 1.00000 ? ? H352 .17941 .19757 .64783 .03800 Uiso ? ? 1.00000 ? ? H353 .11614 .29748 .62156 .05100 Uiso ? ? 1.00000 ? ? H354 .00637 .33933 .72260 .06200 Uiso ? ? 1.00000 ? ? H355 -.03887 .28339 .84994 .05500 Uiso ? ? 1.00000 ? ? H356 .03269 .18606 .88114 .04200 Uiso ? ? 1.00000 ? ? H0a .61931 .18261 .81144 .04500 Uiso ? ? 1.00000 ? ? H0b .61900 .25428 .80068 .04500 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Tl1 .02612(18) .02410(18) .01719(16) -.00020(14) .00263(13) -.00242(14) Tl2 .02841(19) .01504(17) .02224(17) .00425(13) .00391(14) .00111(13) Tl3 .02098(17) .01393(16) .03084(18) .00021(13) .00073(13) .00233(14) Tl4 .0282(2) .0245(2) .0332(2) .00400(15) -.00924(16) -.00239(16) O0 .028(3) .024(3) .016(3) .000(3) .003(3) -.001(2) N11 .013(3) .025(4) .017(3) .003(3) .000(3) -.004(3) N12 .031(4) .020(4) .019(3) .008(3) .003(3) -.002(3) C13 .031(5) .010(4) .021(4) .003(3) .006(4) .002(3) C131 .023(4) .010(4) .022(4) .004(3) .007(3) .006(3) C132 .028(5) .010(4) .029(5) .004(3) .004(4) .000(4) C133 .030(5) .018(5) .028(5) .000(4) .008(4) .006(4) C134 .037(5) .020(5) .022(4) .010(4) .008(4) -.000(4) C135 .053(6) .017(5) .020(4) .003(4) .003(4) -.005(4) C136 .036(5) .018(4) .020(4) .001(4) .003(4) .003(4) C14 .025(5) .021(5) .021(4) -.002(4) -.004(4) -.001(4) C15 .021(4) .014(4) .020(4) .005(3) .002(3) .001(3) C151 .022(4) .014(4) .024(4) -.000(3) -.001(4) .000(3) C152 .033(5) .019(5) .020(4) .004(4) -.002(4) -.006(4) C153 .033(5) .022(5) .032(5) .010(4) -.006(4) -.009(4) C154 .019(5) .030(5) .039(5) .002(4) -.004(4) -.018(4) C155 .030(5) .032(5) .033(5) -.005(4) .013(4) -.006(4) C156 .024(5) .022(5) .028(5) .003(4) .002(4) -.001(4) N21 .034(4) .016(4) .022(4) .001(3) -.000(3) -.004(3) N22 .017(4) .028(4) .019(3) .001(3) -.006(3) -.005(3) C23 .026(4) .012(4) .017(4) -.001(3) .009(3) .001(3) C231 .024(4) .017(4) .022(4) -.002(3) .002(4) -.002(3) C232 .033(5) .031(5) .018(4) -.004(4) .002(4) -.002(4) C233 .020(5) .039(6) .037(5) .005(4) .008(4) -.004(5) C234 .027(5) .045(6) .037(5) -.002(5) -.002(4) -.001(5) C235 .024(5) .029(5) .039(5) -.004(4) -.007(4) -.009(4) C236 .023(5) .020(5) .035(5) .002(4) .004(4) .002(4) C24 .027(5) .018(4) .020(4) -.002(4) -.003(4) -.000(4) C25 .031(5) .022(5) .012(4) -.000(4) -.003(4) .007(3) C251 .023(4) .017(4) .020(4) -.002(3) -.002(4) .004(3) C252 .040(5) .016(4) .015(4) .001(4) -.004(4) -.002(3) C253 .025(5) .027(5) .023(4) .002(4) -.014(4) -.004(4) C254 .038(6) .035(6) .033(5) .015(5) -.006(4) .007(5) C255 .037(6) .022(5) .038(5) .005(4) -.004(5) -.002(4) C256 .033(5) .016(4) .030(5) .000(4) -.004(4) .004(4) N31 .025(4) .018(4) .028(4) .002(3) .005(3) -.002(3) N32 .022(4) .016(4) .025(4) .004(3) .005(3) -.005(3) C33 .024(4) .009(4) .019(4) -.001(3) .005(3) -.004(3) C331 .023(4) .011(4) .021(4) -.003(3) -.006(3) -.005(3) C332 .030(5) .020(5) .025(4) -.005(4) -.001(4) -.005(4) C333 .038(6) .014(4) .036(5) .003(4) -.003(4) -.008(4) C334 .043(6) .026(5) .042(6) -.006(4) -.000(5) .012(5) C335 .031(5) .031(5) .035(5) -.004(4) .003(4) .007(4) C336 .021(4) .023(5) .021(4) -.001(4) -.001(4) -.003(4) C34 .017(4) .020(5) .032(5) .002(3) .001(4) -.008(4) C35 .023(4) .014(4) .021(4) -.004(3) -.003(4) .000(3) C351 .013(4) .016(5) .051(6) -.006(3) -.010(4) .004(4) C352 .018(4) .024(5) .046(6) -.005(4) -.011(4) .002(4) C353 .022(5) .021(5) .076(8) -.013(4) -.016(5) .014(5) C354 .021(5) .017(5) .110(10) -.000(4) -.017(6) .001(6) C355 .023(5) .017(5) .090(9) -.001(4) .002(5) -.008(5) C356 .018(5) .022(5) .058(6) .002(4) .004(4) -.002(5) Cl1 .0330(13) .0435(15) .0342(13) -.0004(11) .0027(11) .0019(11) Cl2 .0507(18) .064(2) .0555(17) -.0151(15) -.0211(14) .0180(16) C0 .046(6) .039(6) .024(5) -.011(5) .006(5) -.002(4) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Tl1 Tl2 . . 4.0801(7) ? Tl1 O0 . . 2.432(6) ? Tl1 N11 . . 2.613(6) ? Tl1 N21 . . 2.933(7) ? Tl1 Tl1 . '3 656' 3.5317(6) ? Tl1 Tl4 . '3 656' 4.0813(6) ? Tl2 N11 . . 3.065(7) ? Tl2 N12 . . 2.737(7) ? Tl2 N21 . . 2.722(7) ? Tl2 N32 . . 2.642(7) ? Tl3 Tl4 . . 3.9679(7) ? Tl3 O0 . . 2.485(6) ? Tl3 N12 . . 2.606(7) ? Tl3 N31 . . 2.648(7) ? Tl4 O0 . . 2.432(6) ? Tl4 N22 . . 2.591(7) ? Tl4 N31 . . 2.905(7) ? O0 H0 . . .851(5) ? N11 N12 . . 1.389(10) ? N11 C15 . . 1.327(10) ? N12 C13 . . 1.363(10) ? C13 C131 . . 1.465(12) ? C13 C14 . . 1.393(12) ? C131 C132 . . 1.389(12) ? C131 C136 . . 1.409(11) ? C132 C133 . . 1.384(12) ? C132 H132 . . .969(8) ? C133 C134 . . 1.367(12) ? C133 H133 . . .969(9) ? C134 C135 . . 1.377(13) ? C134 H134 . . .957(9) ? C135 C136 . . 1.384(13) ? C135 H135 . . .960(9) ? C136 H136 . . .969(9) ? C14 C15 . . 1.413(12) ? C14 H14 . . .963(8) ? C15 C151 . . 1.474(11) ? C151 C152 . . 1.396(12) ? C151 C156 . . 1.381(12) ? C152 C153 . . 1.401(13) ? C152 H152 . . .961(8) ? C153 C154 . . 1.359(13) ? C153 H153 . . .966(9) ? C154 C155 . . 1.404(13) ? C154 H154 . . .955(9) ? C155 C156 . . 1.393(13) ? C155 H155 . . .961(9) ? C156 H156 . . .965(9) ? N21 N22 . . 1.372(10) ? N21 C25 . . 1.367(11) ? N22 C23 . . 1.345(10) ? C23 C231 . . 1.486(11) ? C23 C24 . . 1.404(12) ? C231 C232 . . 1.401(12) ? C231 C236 . . 1.394(12) ? C232 C233 . . 1.381(12) ? C232 H232 . . .962(9) ? C233 C234 . . 1.376(14) ? C233 H233 . . .963(9) ? C234 C235 . . 1.375(14) ? C234 H234 . . .973(9) ? C235 C236 . . 1.391(12) ? C235 H235 . . .971(10) ? C236 H236 . . .964(9) ? C24 C25 . . 1.401(12) ? C24 H24 . . .966(8) ? C25 C251 . . 1.446(12) ? C251 C252 . . 1.410(12) ? C251 C256 . . 1.383(12) ? C252 C253 . . 1.377(12) ? C252 H252 . . .961(8) ? C253 C254 . . 1.363(13) ? C253 H253 . . .968(8) ? C254 C255 . . 1.389(13) ? C254 H254 . . .971(10) ? C255 C256 . . 1.400(13) ? C255 H255 . . .970(9) ? C256 H256 . . .969(9) ? N31 N32 . . 1.380(10) ? N31 C35 . . 1.357(11) ? N32 C33 . . 1.353(11) ? C33 C331 . . 1.493(11) ? C33 C34 . . 1.386(11) ? C331 C332 . . 1.391(12) ? C331 C336 . . 1.401(12) ? C332 C333 . . 1.388(12) ? C332 H332 . . .968(9) ? C333 C334 . . 1.371(14) ? C333 H333 . . .960(9) ? C334 C335 . . 1.371(14) ? C334 H334 . . .974(10) ? C335 C336 . . 1.358(13) ? C335 H335 . . .973(10) ? C336 H336 . . .966(8) ? C34 C35 . . 1.378(12) ? C34 H34 . . .964(8) ? C35 C351 . . 1.475(11) ? C351 C352 . . 1.402(13) ? C351 C356 . . 1.393(13) ? C352 C353 . . 1.397(13) ? C352 H352 . . .960(9) ? C353 C354 . . 1.372(16) ? C353 H353 . . .972(11) ? C354 C355 . . 1.375(17) ? C354 H354 . . .955(10) ? C355 C356 . . 1.396(13) ? C355 H355 . . .967(11) ? C356 H356 . . .966(10) ? Cl1 C0 . . 1.777(9) ? Cl2 C0 . . 1.739(10) ? C0 H0a . . .962(10) ? C0 H0b . . .961(10) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Tl2 Tl1 O0 . . . 71.58(13) ? Tl2 Tl1 N11 . . . 48.66(14) ? Tl2 Tl1 N21 . . . 41.81(14) ? Tl2 Tl1 Tl1 . . '3 656' 103.003(17) ? Tl2 Tl1 Tl4 . . '3 656' 129.172(14) ? O0 Tl1 N11 . . . 82.44(19) ? O0 Tl1 N21 . . . 81.0(2) ? O0 Tl1 Tl1 . . '3 656' 87.75(13) ? O0 Tl1 Tl4 . . '3 656' 149.05(12) ? N11 Tl1 N21 . . . 89.7(2) ? N11 Tl1 Tl1 . . '3 656' 151.66(14) ? N11 Tl1 Tl4 . . '3 656' 128.27(14) ? N21 Tl1 Tl1 . . '3 656' 62.44(14) ? N21 Tl1 Tl4 . . '3 656' 100.63(14) ? Tl1 Tl1 Tl4 '3 656' . '3 656' 66.638(14) ? Tl1 Tl2 N11 . . . 39.81(12) ? Tl1 Tl2 N12 . . . 58.87(14) ? Tl1 Tl2 N21 . . . 45.91(15) ? Tl1 Tl2 N32 . . . 97.61(15) ? N11 Tl2 N12 . . . 26.9(2) ? N11 Tl2 N21 . . . 85.0(2) ? N11 Tl2 N32 . . . 106.4(2) ? N12 Tl2 N21 . . . 103.9(2) ? N12 Tl2 N32 . . . 86.3(2) ? N21 Tl2 N32 . . . 93.0(2) ? Tl4 Tl3 O0 . . . 35.74(13) ? Tl4 Tl3 N12 . . . 95.73(15) ? Tl4 Tl3 N31 . . . 47.04(15) ? O0 Tl3 N12 . . . 80.5(2) ? O0 Tl3 N31 . . . 79.7(2) ? N12 Tl3 N31 . . . 91.1(2) ? Tl3 Tl4 O0 . . . 36.65(13) ? Tl3 Tl4 N22 . . . 103.76(15) ? Tl3 Tl4 N31 . . . 41.85(14) ? Tl3 Tl4 Tl1 . . '3 656' 112.209(15) ? O0 Tl4 N22 . . . 88.9(2) ? O0 Tl4 N31 . . . 75.58(19) ? O0 Tl4 Tl1 . . '3 656' 75.83(13) ? N22 Tl4 N31 . . . 95.2(2) ? N22 Tl4 Tl1 . . '3 656' 58.53(15) ? N31 Tl4 Tl1 . . '3 656' 141.18(14) ? Tl1 O0 Tl3 . . . 121.2(2) ? Tl1 O0 Tl4 . . . 119.8(2) ? Tl1 O0 H0 . . . 92.5(4) ? Tl3 O0 Tl4 . . . 107.6(2) ? Tl3 O0 H0 . . . 117.4(5) ? Tl4 O0 H0 . . . 94.6(4) ? Tl1 N11 Tl2 . . . 91.52(19) ? Tl1 N11 N12 . . . 121.9(4) ? Tl1 N11 C15 . . . 129.4(5) ? Tl2 N11 N12 . . . 63.3(4) ? Tl2 N11 C15 . . . 108.0(5) ? N12 N11 C15 . . . 108.5(6) ? Tl2 N12 Tl3 . . . 109.7(2) ? Tl2 N12 N11 . . . 89.8(4) ? Tl2 N12 C13 . . . 102.2(5) ? Tl3 N12 N11 . . . 118.6(5) ? Tl3 N12 C13 . . . 122.8(5) ? N11 N12 C13 . . . 107.4(6) ? N12 C13 C131 . . . 120.7(7) ? N12 C13 C14 . . . 109.7(7) ? C131 C13 C14 . . . 129.6(7) ? C13 C131 C132 . . . 123.0(7) ? C13 C131 C136 . . . 119.6(7) ? C132 C131 C136 . . . 117.4(7) ? C131 C132 C133 . . . 120.6(8) ? C131 C132 H132 . . . 119.5(8) ? C133 C132 H132 . . . 119.9(8) ? C132 C133 C134 . . . 121.0(8) ? C132 C133 H133 . . . 120.0(8) ? C134 C133 H133 . . . 119.0(9) ? C133 C134 C135 . . . 120.2(8) ? C133 C134 H134 . . . 119.6(9) ? C135 C134 H134 . . . 120.2(8) ? C134 C135 C136 . . . 119.4(8) ? C134 C135 H135 . . . 119.7(9) ? C136 C135 H135 . . . 120.9(9) ? C131 C136 C135 . . . 121.5(8) ? C131 C136 H136 . . . 119.1(8) ? C135 C136 H136 . . . 119.4(8) ? C13 C14 C15 . . . 104.3(7) ? C13 C14 H14 . . . 127.5(8) ? C15 C14 H14 . . . 128.2(8) ? N11 C15 C14 . . . 110.1(7) ? N11 C15 C151 . . . 122.5(7) ? C14 C15 C151 . . . 127.4(7) ? C15 C151 C152 . . . 119.9(7) ? C15 C151 C156 . . . 122.0(7) ? C152 C151 C156 . . . 118.0(8) ? C151 C152 C153 . . . 121.5(8) ? C151 C152 H152 . . . 118.7(8) ? C153 C152 H152 . . . 119.8(8) ? C152 C153 C154 . . . 119.5(8) ? C152 C153 H153 . . . 120.5(9) ? C154 C153 H153 . . . 120.0(9) ? C153 C154 C155 . . . 120.2(8) ? C153 C154 H154 . . . 119.6(9) ? C155 C154 H154 . . . 120.2(9) ? C154 C155 C156 . . . 119.6(8) ? C154 C155 H155 . . . 119.7(9) ? C156 C155 H155 . . . 120.7(9) ? C151 C156 C155 . . . 121.2(8) ? C151 C156 H156 . . . 119.3(8) ? C155 C156 H156 . . . 119.5(9) ? Tl1 N21 Tl2 . . . 92.3(2) ? Tl1 N21 N22 . . . 119.6(5) ? Tl1 N21 C25 . . . 116.2(5) ? Tl2 N21 N22 . . . 94.6(4) ? Tl2 N21 C25 . . . 124.6(5) ? N22 N21 C25 . . . 108.0(7) ? Tl4 N22 N21 . . . 121.4(5) ? Tl4 N22 C23 . . . 121.0(5) ? N21 N22 C23 . . . 108.3(6) ? N22 C23 C231 . . . 122.2(7) ? N22 C23 C24 . . . 110.0(7) ? C231 C23 C24 . . . 127.7(7) ? C23 C231 C232 . . . 121.7(7) ? C23 C231 C236 . . . 120.5(7) ? C232 C231 C236 . . . 117.9(8) ? C231 C232 C233 . . . 120.5(8) ? C231 C232 H232 . . . 119.6(8) ? C233 C232 H232 . . . 119.9(9) ? C232 C233 C234 . . . 120.6(9) ? C232 C233 H233 . . . 119.4(9) ? C234 C233 H233 . . . 120.0(9) ? C233 C234 C235 . . . 120.1(8) ? C233 C234 H234 . . . 120.3(9) ? C235 C234 H234 . . . 119.6(10) ? C234 C235 C236 . . . 119.8(9) ? C234 C235 H235 . . . 121.2(9) ? C236 C235 H235 . . . 119.1(9) ? C231 C236 C235 . . . 121.1(8) ? C231 C236 H236 . . . 119.3(8) ? C235 C236 H236 . . . 119.6(9) ? C23 C24 C25 . . . 104.5(7) ? C23 C24 H24 . . . 128.2(8) ? C25 C24 H24 . . . 127.4(8) ? N21 C25 C24 . . . 109.2(7) ? N21 C25 C251 . . . 122.0(7) ? C24 C25 C251 . . . 128.8(8) ? C25 C251 C252 . . . 122.7(7) ? C25 C251 C256 . . . 120.6(7) ? C252 C251 C256 . . . 116.7(8) ? C251 C252 C253 . . . 122.9(8) ? C251 C252 H252 . . . 118.1(8) ? C253 C252 H252 . . . 119.0(8) ? C252 C253 C254 . . . 118.9(8) ? C252 C253 H253 . . . 120.3(8) ? C254 C253 H253 . . . 120.8(9) ? C253 C254 C255 . . . 120.5(9) ? C253 C254 H254 . . . 119.0(9) ? C255 C254 H254 . . . 120.5(9) ? C254 C255 C256 . . . 120.0(9) ? C254 C255 H255 . . . 120.4(9) ? C256 C255 H255 . . . 119.7(9) ? C251 C256 C255 . . . 120.8(8) ? C251 C256 H256 . . . 119.3(8) ? C255 C256 H256 . . . 120.0(9) ? Tl3 N31 Tl4 . . . 91.1(2) ? Tl3 N31 N32 . . . 119.7(5) ? Tl3 N31 C35 . . . 119.5(5) ? Tl4 N31 N32 . . . 86.1(4) ? Tl4 N31 C35 . . . 128.5(5) ? N32 N31 C35 . . . 108.1(7) ? Tl2 N32 N31 . . . 129.1(5) ? Tl2 N32 C33 . . . 115.7(5) ? N31 N32 C33 . . . 107.0(6) ? N32 C33 C331 . . . 120.9(7) ? N32 C33 C34 . . . 110.0(7) ? C331 C33 C34 . . . 129.1(7) ? C33 C331 C332 . . . 122.0(7) ? C33 C331 C336 . . . 120.0(7) ? C332 C331 C336 . . . 118.0(7) ? C331 C332 C333 . . . 121.5(8) ? C331 C332 H332 . . . 119.2(8) ? C333 C332 H332 . . . 119.3(9) ? C332 C333 C334 . . . 118.5(8) ? C332 C333 H333 . . . 120.1(9) ? C334 C333 H333 . . . 121.4(9) ? C333 C334 C335 . . . 120.6(9) ? C333 C334 H334 . . . 119.4(9) ? C335 C334 H334 . . . 120.0(10) ? C334 C335 C336 . . . 121.2(9) ? C334 C335 H335 . . . 119.6(9) ? C336 C335 H335 . . . 119.2(9) ? C331 C336 C335 . . . 120.1(8) ? C331 C336 H336 . . . 119.4(8) ? C335 C336 H336 . . . 120.5(9) ? C33 C34 C35 . . . 105.4(7) ? C33 C34 H34 . . . 127.3(8) ? C35 C34 H34 . . . 127.3(8) ? N31 C35 C34 . . . 109.4(7) ? N31 C35 C351 . . . 121.9(7) ? C34 C35 C351 . . . 128.6(8) ? C35 C351 C352 . . . 122.4(8) ? C35 C351 C356 . . . 120.2(8) ? C352 C351 C356 . . . 117.4(8) ? C351 C352 C353 . . . 120.7(9) ? C351 C352 H352 . . . 119.7(9) ? C353 C352 H352 . . . 119.7(10) ? C352 C353 C354 . . . 120.3(10) ? C352 C353 H353 . . . 119.4(10) ? C354 C353 H353 . . . 120.3(9) ? C353 C354 C355 . . . 120.4(9) ? C353 C354 H354 . . . 120.4(12) ? C355 C354 H354 . . . 119.1(11) ? C354 C355 C356 . . . 119.4(10) ? C354 C355 H355 . . . 120.7(9) ? C356 C355 H355 . . . 119.9(11) ? C351 C356 C355 . . . 121.7(9) ? C351 C356 H356 . . . 118.6(9) ? C355 C356 H356 . . . 119.6(10) ? Cl1 C0 Cl2 . . . 111.9(5) ? Cl1 C0 H0a . . . 109.2(7) ? Cl1 C0 H0b . . . 109.2(7) ? Cl2 C0 H0a . . . 109.4(8) ? Cl2 C0 H0b . . . 109.5(8) ? H0a C0 H0b . . . 107.6(9) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Tl1 Tl3 4.2841(7) . . ? Tl1 Tl4 4.2070(8) . . ? Tl1 N12 3.548(7) . . ? Tl1 C15 3.605(8) . . ? Tl1 C151 3.861(8) . . ? Tl1 C156 3.576(8) . . ? Tl1 N21 3.390(7) . '3 656' ? Tl1 N22 3.511(7) . '3 656' ? Tl1 N22 3.802(7) . . ? Tl1 C23 3.606(8) . '3 656' ? Tl1 C24 3.562(8) . '3 656' ? Tl1 C25 3.743(9) . . ? Tl1 C25 3.411(8) . '3 656' ? Tl1 C251 3.896(8) . . ? Tl1 C251 3.987(8) . '3 656' ? Tl1 C252 3.477(8) . . ? Tl1 Cl1 3.862(3) . . ? Tl1 H0 2.6110(4) . . ? Tl1 H156 3.0403(5) . . ? Tl1 H252 2.9696(5) . . ? Tl2 Tl3 4.3674(9) . . ? Tl2 Tl4 4.4490(8) . . ? Tl2 O0 4.036(6) . . ? Tl2 C13 3.305(8) . . ? Tl2 C131 3.934(8) . . ? Tl2 C132 3.804(8) . . ? Tl2 C135 3.918(9) . '3 657' ? Tl2 C136 3.601(8) . '3 657' ? Tl2 C14 3.862(8) . . ? Tl2 C15 3.696(8) . . ? Tl2 N22 3.146(7) . . ? Tl2 C23 4.167(8) . . ? Tl2 C25 3.675(8) . . ? Tl2 C252 4.080(9) . . ? Tl2 N31 3.671(7) . . ? Tl2 C33 3.450(8) . . ? Tl2 C331 3.548(8) . . ? Tl2 C332 3.274(9) . . ? Tl2 C333 4.144(9) . . ? Tl2 H132 3.1704(5) . . ? Tl2 H136 3.4054(6) . '3 657' ? Tl2 H14 3.5647(7) . '3 657' ? Tl2 H252 3.3068(5) . . ? Tl2 H332 2.9081(5) . . ? Tl3 N11 3.491(7) . . ? Tl3 C13 3.535(8) . . ? Tl3 C131 3.796(8) . . ? Tl3 C132 3.590(9) . . ? Tl3 C134 4.041(9) . '4 554' ? Tl3 C135 3.921(9) . '4 554' ? Tl3 C255 3.878(9) . '2 656' ? Tl3 C256 4.125(9) . '2 656' ? Tl3 N32 3.541(7) . . ? Tl3 C35 3.520(8) . . ? Tl3 C351 3.783(8) . . ? Tl3 C352 3.554(9) . . ? Tl3 Cl1 3.611(2) . . ? Tl3 C0 3.857(10) . . ? Tl3 H0 2.9739(6) . . ? Tl3 H132 3.1134(6) . . ? Tl3 H134 3.6136(6) . '4 554' ? Tl3 H135 3.3736(6) . '4 554' ? Tl3 H352 3.0688(5) . . ? Tl3 H0a 3.4647(6) . . ? Tl4 N21 3.507(7) . . ? Tl4 C23 3.481(8) . . ? Tl4 C231 3.720(8) . . ? Tl4 C232 3.450(9) . . ? Tl4 C233 4.163(9) . '3 556' ? Tl4 C234 3.950(9) . '3 556' ? Tl4 C252 4.077(8) . '3 656' ? Tl4 C253 3.824(8) . '3 656' ? Tl4 C254 3.855(10) . '3 656' ? Tl4 C255 4.174(9) . '3 656' ? Tl4 N32 3.130(7) . . ? Tl4 C33 4.146(8) . . ? Tl4 C35 3.896(8) . . ? Tl4 H0 2.6395(5) . . ? Tl4 H232 2.9938(5) . . ? Tl4 H233 3.6289(6) . '3 556' ? Tl4 H234 3.2038(5) . '3 556' ? Tl4 H352 3.5579(6) . . ? O0 Cl1 3.856(6) . . ? N11 C13 2.217(10) . . ? N11 C14 2.247(10) . . ? N11 C151 2.457(10) . . ? N11 Cl1 3.503(7) . . ? N12 C131 2.458(10) . . ? N12 C132 2.962(11) . . ? N12 C14 2.253(11) . . ? N12 C15 2.204(11) . . ? N12 Cl1 3.849(7) . . ? C13 C132 2.509(12) . . ? C13 C136 2.484(12) . . ? C13 C15 2.217(12) . . ? C13 H14 2.122(8) . . ? C131 C133 2.410(12) . . ? C131 C134 2.796(12) . . ? C131 C135 2.437(12) . . ? C131 C14 2.587(12) . . ? C131 H132 2.048(8) . . ? C131 H136 2.062(8) . . ? C132 C134 2.394(12) . . ? C132 C135 2.771(12) . . ? C132 C136 2.391(12) . . ? C132 H133 2.049(9) . . ? C133 C135 2.378(13) . . ? C133 C136 2.743(12) . . ? C133 H132 2.047(9) . . ? C133 H134 2.019(9) . . ? C134 C136 2.384(13) . . ? C134 H133 2.023(9) . . ? C134 H135 2.031(9) . . ? C135 Cl1 3.686(10) . 4 ? C135 H134 2.035(10) . . ? C135 H136 2.043(10) . . ? C136 Cl1 3.870(9) . 4 ? C136 H135 2.050(8) . . ? C14 C151 2.589(12) . . ? C15 C152 2.485(12) . . ? C15 C156 2.498(12) . . ? C15 Cl2 3.923(8) . . ? C15 H14 2.146(8) . . ? C151 C153 2.440(12) . . ? C151 C154 2.801(12) . . ? C151 C155 2.416(13) . . ? C151 H152 2.039(8) . . ? C151 H156 2.035(8) . . ? C152 C154 2.385(13) . . ? C152 C155 2.757(13) . . ? C152 C156 2.380(12) . . ? C152 H153 2.066(9) . . ? C153 C155 2.396(13) . . ? C153 C156 2.776(12) . . ? C153 H152 2.056(9) . . ? C153 H154 2.010(9) . . ? C154 C156 2.417(12) . . ? C154 H153 2.024(9) . . ? C154 H155 2.057(9) . . ? C155 H154 2.057(9) . . ? C155 H156 2.048(9) . . ? C156 Cl2 3.827(9) . . ? C156 H155 2.058(9) . . ? N21 C23 2.202(11) . . ? N21 C24 2.256(11) . . ? N21 C251 2.460(11) . . ? N21 C252 2.945(11) . . ? N22 C231 2.479(10) . . ? N22 C232 2.983(11) . . ? N22 C24 2.253(11) . . ? N22 C25 2.216(11) . . ? C23 C232 2.521(12) . . ? C23 C236 2.500(12) . . ? C23 C25 2.217(12) . . ? C23 H24 2.139(8) . . ? C231 C233 2.416(12) . . ? C231 C234 2.794(12) . . ? C231 C235 2.425(12) . . ? C231 C24 2.594(12) . . ? C231 H232 2.054(8) . . ? C231 H236 2.047(8) . . ? C232 C234 2.395(13) . . ? C232 C235 2.768(13) . . ? C232 C236 2.394(13) . . ? C232 H233 2.035(9) . . ? C233 C235 2.383(14) . . ? C233 C236 2.755(13) . . ? C233 H232 2.039(9) . . ? C233 H234 2.047(9) . . ? C234 C236 2.392(13) . . ? C234 H233 2.036(10) . . ? C234 H235 2.053(10) . . ? C235 H234 2.040(9) . . ? C235 H236 2.047(9) . . ? C236 Cl1 3.747(9) . '3 656' ? C236 H235 2.047(9) . . ? C24 C251 2.567(12) . . ? C24 Cl1 3.618(9) . '3 656' ? C24 Cl2 3.936(9) . '2 646' ? C25 C252 2.507(12) . . ? C25 C256 2.458(12) . . ? C25 H24 2.130(8) . . ? C251 C253 2.448(12) . . ? C251 C254 2.802(13) . . ? C251 C255 2.420(12) . . ? C251 H252 2.047(8) . . ? C251 H256 2.040(8) . . ? C252 C254 2.359(13) . . ? C252 C255 2.734(13) . . ? C252 C256 2.378(12) . . ? C252 H253 2.043(9) . . ? C253 C255 2.389(13) . . ? C253 C256 2.782(12) . . ? C253 H252 2.025(9) . . ? C253 H254 2.020(9) . . ? C254 C256 2.415(13) . . ? C254 H253 2.036(10) . . ? C254 H255 2.057(10) . . ? C255 H254 2.059(9) . . ? C255 H256 2.062(9) . . ? C256 H0 2.467(9) . '3 656' ? C256 H255 2.060(9) . . ? N31 C33 2.197(10) . . ? N31 C34 2.233(11) . . ? N31 C351 2.476(11) . . ? N31 C352 2.975(11) . . ? N32 C331 2.476(11) . . ? N32 C332 2.987(11) . . ? N32 C34 2.244(11) . . ? N32 C35 2.216(10) . . ? C33 C332 2.523(12) . . ? C33 C336 2.507(11) . . ? C33 C35 2.198(11) . . ? C33 H34 2.114(8) . . ? C331 C333 2.425(12) . . ? C331 C334 2.770(12) . . ? C331 C335 2.390(12) . . ? C331 C34 2.599(11) . . ? C331 H332 2.046(8) . . ? C331 H336 2.056(8) . . ? C332 C334 2.372(13) . . ? C332 C335 2.734(13) . . ? C332 C336 2.393(12) . . ? C332 H333 2.046(9) . . ? C333 C335 2.382(13) . . ? C333 C336 2.774(12) . . ? C333 Cl1 3.938(9) . '2 646' ? C333 Cl2 3.808(10) . '2 646' ? C333 H332 2.045(9) . . ? C333 H334 2.035(9) . . ? C334 C336 2.378(13) . . ? C334 Cl2 3.881(11) . '3 657' ? C334 H333 2.043(10) . . ? C334 H335 2.035(10) . . ? C335 H334 2.040(10) . . ? C335 H336 2.027(10) . . ? C336 H335 2.020(8) . . ? C34 C351 2.571(12) . . ? C35 C352 2.521(12) . . ? C35 C356 2.486(12) . . ? C35 H34 2.107(8) . . ? C351 C353 2.432(13) . . ? C351 C354 2.805(13) . . ? C351 C355 2.437(13) . . ? C351 H352 2.054(9) . . ? C351 H356 2.041(9) . . ? C352 C354 2.402(13) . . ? C352 C355 2.773(14) . . ? C352 C356 2.388(14) . . ? C352 H353 2.057(9) . . ? C353 C355 2.384(16) . . ? C353 C356 2.756(15) . . ? C353 H352 2.049(9) . . ? C353 H354 2.031(10) . . ? C354 C356 2.393(15) . . ? C354 H353 2.043(13) . . ? C354 H355 2.045(13) . . ? C355 Cl2 3.425(10) . '1 455' ? C355 H354 2.021(11) . . ? C355 H356 2.053(10) . . ? C356 Cl2 3.839(9) . '1 455' ? C356 H355 2.057(9) . . ? Cl1 Cl2 2.914(4) . . ? Cl1 H135 3.099(3) . '4 554' ? Cl1 H136 3.433(3) . '4 554' ? Cl1 H156 3.268(3) . . ? Cl1 H236 2.847(2) . '3 656' ? Cl1 H24 3.068(2) . '3 656' ? Cl1 H333 3.112(3) . '2 656' ? Cl1 H0a 2.281(2) . . ? Cl1 H0b 2.281(2) . . ? Cl2 H333 2.906(3) . '2 656' ? Cl2 H334 3.230(3) . '3 657' ? Cl2 H355 3.031(3) . '1 655' ? Cl2 H0a 2.249(3) . . ? Cl2 H0b 2.251(3) . . ? H0a H0b 1.5514(3) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2880 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 29 _reflns_limit_l_min -20 _reflns_limit_l_max 20 _reflns_number_observed ? _reflns_d_resolution_high .728 _reflns_d_resolution_low 13.803 _diffrn_reflns_av_sigmaI/netI .1 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .066 _refine_ls_wR_factor_all .047 _refine_ls_goodness_of_fit_all .95 _refine_ls_shift/su_mean .004 data_tlmppz # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C30.5 H29 Cl1 N6 O1 Tl4' _chemical_formula_moiety ? _chemical_formula_weight 1348.59 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 7.3310(10) _cell_length_b 26.592(5) _cell_length_c 18.044(3) _cell_angle_alpha 90.00000 _cell_angle_beta 97.516(3) _cell_angle_gamma 90.00000 _cell_volume 3487.4(10) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.569 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 18.535 _exptl_crystal_description flake _exptl_crystal_size_max .12 _exptl_crystal_size_mid .08 _exptl_crystal_size_min .03 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .343 _exptl_absorpt_correction_T_max .894 _diffrn_reflns_number 40698 _reflns_number_total 6010 _reflns_Friedel_coverage 0 _reflns_number_gt 4469 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 24.79 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .101 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .067 _refine_ls_wR_factor_ref .087 _refine_ls_goodness_of_fit_ref 1.936 _refine_ls_number_reflns 4469 _refine_ls_number_parameters 208 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .012 _refine_diff_density_min -2.872 _refine_diff_density_max 4.49 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 4269(283) _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 122 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 116 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 4 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 24 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Tl ? 0 16 -3.556 9.659 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Tl1 .80268(14) .33574(4) .80371(5) .0302(6) Uani ? ? 1.00000 ? ? Tl2 .27401(14) .30123(4) .88427(6) .0346(6) Uani ? ? 1.00000 ? ? Tl3 .30653(15) .34913(5) .67106(6) .0393(7) Uani ? ? 1.00000 ? ? Tl4 .45947(15) .20138(4) .75010(6) .0346(6) Uani ? ? 1.00000 ? ? O0 .273(2) .2781(7) .7523(10) .038(5) Uiso ? ? 1.00000 ? ? N11 .618(3) .3037(9) .6519(13) .042(6) Uiso ? ? 1.00000 ? ? N12 .685(3) .2646(8) .6965(11) .032(5) Uiso ? ? 1.00000 ? ? C13 .825(3) .2436(10) .6648(13) .028(6) Uiso ? ? 1.00000 ? ? C131 .917(4) .1986(10) .6955(14) .032(6) Uiso ? ? 1.00000 ? ? C132 .933(4) .1851(11) .7720(14) .036(7) Uiso ? ? 1.00000 ? ? C133 1.015(4) .1424(11) .7997(15) .039(7) Uiso ? ? 1.00000 ? ? C134 1.093(4) .1091(13) .7488(16) .051(8) Uiso ? ? 1.00000 ? ? C135 1.086(4) .1222(12) .6739(16) .046(8) Uiso ? ? 1.00000 ? ? C136 1.004(4) .1655(11) .6499(14) .035(7) Uiso ? ? 1.00000 ? ? C14 .848(4) .2725(11) .6002(14) .034(7) Uiso ? ? 1.00000 ? ? C15 .722(4) .3072(11) .5956(15) .038(7) Uiso ? ? 1.00000 ? ? C151 .678(4) .3465(13) .5336(17) .052(8) Uiso ? ? 1.00000 ? ? N21 .600(3) .2348(9) .8829(11) .034(5) Uiso ? ? 1.00000 ? ? N22 .644(3) .2846(8) .8973(11) .028(5) Uiso ? ? 1.00000 ? ? C23 .746(3) .2869(10) .9672(13) .026(6) Uiso ? ? 1.00000 ? ? C231 .812(3) .3349(10) .9980(12) .024(5) Uiso ? ? 1.00000 ? ? C232 .727(4) .3806(11) .9776(14) .032(6) Uiso ? ? 1.00000 ? ? C233 .795(4) .4251(10) 1.0062(13) .032(6) Uiso ? ? 1.00000 ? ? C234 .953(4) .4270(11) 1.0590(14) .035(7) Uiso ? ? 1.00000 ? ? C235 1.036(4) .3822(11) 1.0785(14) .035(7) Uiso ? ? 1.00000 ? ? C236 .975(3) .3384(9) 1.0474(11) .018(5) Uiso ? ? 1.00000 ? ? C24 .768(4) .2373(11) .9943(15) .039(7) Uiso ? ? 1.00000 ? ? C25 .673(4) .2067(10) .9402(14) .032(6) Uiso ? ? 1.00000 ? ? C251 .640(4) .1533(13) .9384(17) .052(8) Uiso ? ? 1.00000 ? ? N31 .368(3) .3856(8) .8296(11) .032(5) Uiso ? ? 1.00000 ? ? N32 .511(3) .3945(8) .7894(11) .030(5) Uiso ? ? 1.00000 ? ? C33 .549(3) .4445(10) .7909(13) .029(6) Uiso ? ? 1.00000 ? ? C331 .696(4) .4665(11) .7551(14) .035(6) Uiso ? ? 1.00000 ? ? C332 .777(4) .4397(11) .7004(15) .042(7) Uiso ? ? 1.00000 ? ? C333 .927(4) .4590(12) .6682(15) .041(7) Uiso ? ? 1.00000 ? ? C334 .992(5) .5071(14) .6928(18) .061(9) Uiso ? ? 1.00000 ? ? C335 .907(4) .5335(13) .7447(17) .053(9) Uiso ? ? 1.00000 ? ? C336 .767(4) .5130(11) .7749(14) .038(7) Uiso ? ? 1.00000 ? ? C34 .419(4) .4685(11) .8312(14) .035(7) Uiso ? ? 1.00000 ? ? C35 .314(4) .4304(11) .8533(14) .034(6) Uiso ? ? 1.00000 ? ? C351 .150(4) .4347(11) .8985(15) .041(7) Uiso ? ? 1.00000 ? ? Cl1 .579(8) .519(3) .544(4) .36(9) Uani ? ? .50000 ? ? Cl2 .288(9) .483(2) .531(4) .29(7) Uani ? ? .50000 ? ? C0 .374(17) .522(5) .587(6) .12(4) Uiso ? ? .50000 ? ? H132 .88496 .20873 .80576 .04700 Uiso ? ? 1.00000 ? ? H133 1.02058 .13399 .85251 .05400 Uiso ? ? 1.00000 ? ? H134 1.14863 .07766 .76597 .06300 Uiso ? ? 1.00000 ? ? H135 1.14343 .10030 .63921 .05700 Uiso ? ? 1.00000 ? ? H136 1.00275 .17523 .59768 .04600 Uiso ? ? 1.00000 ? ? H14 .93997 .26743 .56606 .04200 Uiso ? ? 1.00000 ? ? H232 .61662 .38019 .94208 .04100 Uiso ? ? 1.00000 ? ? H233 .73174 .45592 .98988 .04000 Uiso ? ? 1.00000 ? ? H234 .99982 .45929 1.08016 .04600 Uiso ? ? 1.00000 ? ? H235 1.14154 .38288 1.11640 .04800 Uiso ? ? 1.00000 ? ? H236 1.04641 .30820 1.05885 .02400 Uiso ? ? 1.00000 ? ? H24 .83578 .22680 1.04259 .05100 Uiso ? ? 1.00000 ? ? H332 .72828 .40671 .68436 .05300 Uiso ? ? 1.00000 ? ? H333 .98313 .44041 .63141 .05400 Uiso ? ? 1.00000 ? ? H334 1.09618 .52211 .67238 .08100 Uiso ? ? 1.00000 ? ? H335 .95018 .56703 .76081 .07200 Uiso ? ? 1.00000 ? ? H336 .70829 .53224 .81189 .04800 Uiso ? ? 1.00000 ? ? H34 .41166 .50467 .84090 .04600 Uiso ? ? 1.00000 ? ? H151a .76275 .34544 .49794 .07900 Uiso ? ? 1.00000 ? ? H151b .68358 .38026 .55490 .07900 Uiso ? ? 1.00000 ? ? H151c .55625 .34209 .50817 .07900 Uiso ? ? 1.00000 ? ? H251a .68381 .13801 .98598 .07600 Uiso ? ? 1.00000 ? ? H251b .70499 .13715 .90157 .07600 Uiso ? ? 1.00000 ? ? H251c .51304 .14593 .92667 .07600 Uiso ? ? 1.00000 ? ? H351a .12496 .46938 .90901 .06300 Uiso ? ? 1.00000 ? ? H351b .17464 .41734 .94497 .06300 Uiso ? ? 1.00000 ? ? H351c .04066 .42081 .87112 .06300 Uiso ? ? 1.00000 ? ? H0 .14696 .27360 .74560 .05000 Uiso ? ? 1.00000 ? ? H0a .31358 .55772 .58444 .15400 Uiso ? ? .50000 ? ? H0b .38316 .51607 .64142 .15400 Uiso ? ? .50000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Tl1 .0226(6) .0342(7) .0325(6) .0017(5) -.0014(4) -.0024(5) Tl2 .0267(6) .0384(7) .0388(6) .0028(5) .0046(4) .0007(5) Tl3 .0350(7) .0475(8) .0321(6) .0093(5) -.0088(5) -.0062(5) Tl4 .0303(6) .0353(7) .0383(6) -.0051(5) .0053(5) -.0099(5) Cl1 .17(5) .50(12) .38(9) -.09(6) -.05(5) .18(9) Cl2 .35(8) .25(7) .28(7) .01(6) .11(6) .03(6) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Tl1 Tl3 . . 4.0997(15) ? Tl1 N11 . . 3.01(2) ? Tl1 N12 . . 2.76(2) ? Tl1 N22 . . 2.56(2) ? Tl1 N32 . . 2.63(2) ? Tl1 Tl2 . '1 655' 3.6852(15) ? Tl2 Tl3 . . 4.0891(16) ? Tl2 Tl4 . . 3.9524(17) ? Tl2 O0 . . 2.459(18) ? Tl2 N21 . . 2.97(2) ? Tl2 N22 . . 2.73(2) ? Tl2 N31 . . 2.58(2) ? Tl3 O0 . . 2.422(19) ? Tl3 N11 . . 2.65(2) ? Tl3 N31 . . 3.00(2) ? Tl3 N32 . . 2.72(2) ? Tl4 O0 . . 2.46(2) ? Tl4 N12 . . 2.63(2) ? Tl4 N21 . . 2.63(2) ? O0 H0 . . .927(18) ? N11 N12 . . 1.36(3) ? N11 C15 . . 1.35(4) ? N12 C13 . . 1.36(3) ? C13 C131 . . 1.45(4) ? C13 C14 . . 1.43(4) ? C131 C132 . . 1.42(4) ? C131 C136 . . 1.41(4) ? C132 C133 . . 1.35(4) ? C132 H132 . . .97(3) ? C133 C134 . . 1.44(4) ? C133 H133 . . .97(3) ? C134 C135 . . 1.39(4) ? C134 H134 . . .96(3) ? C135 C136 . . 1.34(4) ? C135 H135 . . .99(3) ? C136 H136 . . .98(3) ? C14 C15 . . 1.31(4) ? C14 H14 . . .98(3) ? C15 C151 . . 1.53(4) ? C151 H151a . . .95(3) ? C151 H151b . . .98(3) ? C151 H151c . . .96(3) ? N21 N22 . . 1.38(3) ? N21 C25 . . 1.33(3) ? N22 C23 . . 1.38(3) ? C23 C231 . . 1.45(4) ? C23 C24 . . 1.41(4) ? C231 C232 . . 1.39(4) ? C231 C236 . . 1.40(3) ? C232 C233 . . 1.36(4) ? C232 H232 . . .97(2) ? C233 C234 . . 1.40(3) ? C233 H233 . . .97(3) ? C234 C235 . . 1.36(4) ? C234 H234 . . .98(3) ? C235 C236 . . 1.34(4) ? C235 H235 . . .97(2) ? C236 H236 . . .97(2) ? C24 C25 . . 1.38(4) ? C24 H24 . . .99(3) ? C25 C251 . . 1.44(4) ? C251 H251a . . .97(3) ? C251 H251b . . .97(3) ? C251 H251c . . .95(3) ? N31 N32 . . 1.37(3) ? N31 C35 . . 1.34(4) ? N32 C33 . . 1.36(3) ? C33 C331 . . 1.45(4) ? C33 C34 . . 1.42(4) ? C331 C332 . . 1.41(4) ? C331 C336 . . 1.37(4) ? C332 C333 . . 1.41(4) ? C332 H332 . . .97(3) ? C333 C334 . . 1.42(5) ? C333 H333 . . .96(3) ? C334 C335 . . 1.38(5) ? C334 H334 . . .98(4) ? C335 C336 . . 1.34(4) ? C335 H335 . . .98(3) ? C336 H336 . . .98(3) ? C34 C35 . . 1.36(4) ? C34 H34 . . .98(3) ? C35 C351 . . 1.54(4) ? C351 H351a . . .96(3) ? C351 H351b . . .95(3) ? C351 H351c . . .96(3) ? Cl1 C0 . . 1.78(14) ? Cl1 Cl1 . '3 666' 2.10(10) ? Cl1 Cl2 . '3 666' 1.77(10) ? Cl2 C0 . . 1.53(13) ? C0 H0a . . 1.04(13) ? C0 H0b . . .99(11) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Tl3 Tl1 N11 . . . 40.2(5) ? Tl3 Tl1 N12 . . . 58.6(4) ? Tl3 Tl1 N22 . . . 89.2(4) ? Tl3 Tl1 N32 . . . 40.9(4) ? Tl3 Tl1 Tl2 . . '1 655' 165.10(4) ? N11 Tl1 N12 . . . 26.9(6) ? N11 Tl1 N22 . . . 105.1(6) ? N11 Tl1 N32 . . . 79.4(6) ? N11 Tl1 Tl2 . . '1 655' 125.0(5) ? N12 Tl1 N22 . . . 88.4(6) ? N12 Tl1 N32 . . . 99.4(6) ? N12 Tl1 Tl2 . . '1 655' 107.2(4) ? N22 Tl1 N32 . . . 86.9(7) ? N22 Tl1 Tl2 . . '1 655' 95.3(4) ? N32 Tl1 Tl2 . . '1 655' 153.4(4) ? Tl3 Tl2 Tl4 . . . 64.27(3) ? Tl3 Tl2 O0 . . . 32.8(5) ? Tl3 Tl2 N21 . . . 91.8(4) ? Tl3 Tl2 N22 . . . 87.2(4) ? Tl3 Tl2 N31 . . . 47.0(4) ? Tl3 Tl2 Tl1 . . '1 455' 73.64(3) ? Tl4 Tl2 O0 . . . 36.5(4) ? Tl4 Tl2 N21 . . . 41.8(4) ? Tl4 Tl2 N22 . . . 61.7(4) ? Tl4 Tl2 N31 . . . 102.7(5) ? Tl4 Tl2 Tl1 . . '1 455' 107.79(3) ? O0 Tl2 N21 . . . 75.1(6) ? O0 Tl2 N22 . . . 85.3(6) ? O0 Tl2 N31 . . . 79.3(6) ? O0 Tl2 Tl1 . . '1 455' 78.3(4) ? N21 Tl2 N22 . . . 27.6(6) ? N21 Tl2 N31 . . . 105.0(6) ? N21 Tl2 Tl1 . . '1 455' 149.0(4) ? N22 Tl2 N31 . . . 82.0(6) ? N22 Tl2 Tl1 . . '1 455' 160.9(4) ? N31 Tl2 Tl1 . . '1 455' 85.2(5) ? Tl1 Tl3 Tl2 . . . 65.17(3) ? Tl1 Tl3 O0 . . . 74.4(4) ? Tl1 Tl3 N11 . . . 47.3(5) ? Tl1 Tl3 N31 . . . 57.3(4) ? Tl1 Tl3 N32 . . . 39.2(4) ? Tl2 Tl3 O0 . . . 33.4(4) ? Tl2 Tl3 N11 . . . 97.9(5) ? Tl2 Tl3 N31 . . . 39.0(4) ? Tl2 Tl3 N32 . . . 59.6(5) ? O0 Tl3 N11 . . . 83.1(7) ? O0 Tl3 N31 . . . 71.9(6) ? O0 Tl3 N32 . . . 87.7(6) ? N11 Tl3 N31 . . . 104.3(6) ? N11 Tl3 N32 . . . 84.7(7) ? N31 Tl3 N32 . . . 27.2(6) ? Tl2 Tl4 O0 . . . 36.5(4) ? Tl2 Tl4 N12 . . . 94.5(5) ? Tl2 Tl4 N21 . . . 48.8(5) ? O0 Tl4 N12 . . . 81.5(7) ? O0 Tl4 N21 . . . 81.8(6) ? N12 Tl4 N21 . . . 86.0(6) ? Tl2 O0 Tl3 . . . 113.8(8) ? Tl2 O0 Tl4 . . . 107.0(6) ? Tl2 O0 H0 . . . 91.9(12) ? Tl3 O0 Tl4 . . . 122.6(8) ? Tl3 O0 H0 . . . 101.5(13) ? Tl4 O0 H0 . . . 116.0(15) ? Tl1 N11 Tl3 . . . 92.5(7) ? Tl1 N11 N12 . . . 66.2(12) ? Tl1 N11 C15 . . . 115.9(17) ? Tl3 N11 N12 . . . 121.3(17) ? Tl3 N11 C15 . . . 130.2(18) ? N12 N11 C15 . . . 108(2) ? Tl1 N12 Tl4 . . . 109.5(7) ? Tl1 N12 N11 . . . 87.0(14) ? Tl1 N12 C13 . . . 113.2(15) ? Tl4 N12 N11 . . . 120.6(16) ? Tl4 N12 C13 . . . 115.9(16) ? N11 N12 C13 . . . 107(2) ? N12 C13 C131 . . . 121(2) ? N12 C13 C14 . . . 108(2) ? C131 C13 C14 . . . 131(2) ? C13 C131 C132 . . . 124(2) ? C13 C131 C136 . . . 121(2) ? C132 C131 C136 . . . 115(2) ? C131 C132 C133 . . . 123(3) ? C131 C132 H132 . . . 117(3) ? C133 C132 H132 . . . 119(3) ? C132 C133 C134 . . . 118(3) ? C132 C133 H133 . . . 121(3) ? C134 C133 H133 . . . 121(3) ? C133 C134 C135 . . . 120(3) ? C133 C134 H134 . . . 121(3) ? C135 C134 H134 . . . 119(3) ? C134 C135 C136 . . . 119(3) ? C134 C135 H135 . . . 120(3) ? C136 C135 H135 . . . 121(3) ? C131 C136 C135 . . . 124(3) ? C131 C136 H136 . . . 117(3) ? C135 C136 H136 . . . 119(3) ? C13 C14 C15 . . . 106(2) ? C13 C14 H14 . . . 127(3) ? C15 C14 H14 . . . 127(3) ? N11 C15 C14 . . . 112(3) ? N11 C15 C151 . . . 121(3) ? C14 C15 C151 . . . 127(3) ? C15 C151 H151a . . . 112(3) ? C15 C151 H151b . . . 110(3) ? C15 C151 H151c . . . 111(3) ? H151a C151 H151b . . . 107(3) ? H151a C151 H151c . . . 109(3) ? H151b C151 H151c . . . 107(3) ? Tl2 N21 Tl4 . . . 89.4(6) ? Tl2 N21 N22 . . . 66.2(12) ? Tl2 N21 C25 . . . 124.7(17) ? Tl4 N21 N22 . . . 123.2(14) ? Tl4 N21 C25 . . . 126.1(18) ? N22 N21 C25 . . . 109(2) ? Tl1 N22 Tl2 . . . 113.0(7) ? Tl1 N22 N21 . . . 120.0(15) ? Tl1 N22 C23 . . . 109.8(15) ? Tl2 N22 N21 . . . 86.2(13) ? Tl2 N22 C23 . . . 119.0(16) ? N21 N22 C23 . . . 107(2) ? N22 C23 C231 . . . 120(2) ? N22 C23 C24 . . . 107(2) ? C231 C23 C24 . . . 132(2) ? C23 C231 C232 . . . 124(2) ? C23 C231 C236 . . . 121(2) ? C232 C231 C236 . . . 115(2) ? C231 C232 C233 . . . 122(2) ? C231 C232 H232 . . . 118(3) ? C233 C232 H232 . . . 120(3) ? C232 C233 C234 . . . 121(2) ? C232 C233 H233 . . . 119(2) ? C234 C233 H233 . . . 120(3) ? C233 C234 C235 . . . 116(2) ? C233 C234 H234 . . . 121(3) ? C235 C234 H234 . . . 123(2) ? C234 C235 C236 . . . 123(2) ? C234 C235 H235 . . . 117(3) ? C236 C235 H235 . . . 120(3) ? C231 C236 C235 . . . 122(2) ? C231 C236 H236 . . . 118(2) ? C235 C236 H236 . . . 120(2) ? C23 C24 C25 . . . 106(2) ? C23 C24 H24 . . . 126(3) ? C25 C24 H24 . . . 127(3) ? N21 C25 C24 . . . 110(2) ? N21 C25 C251 . . . 119(2) ? C24 C25 C251 . . . 131(2) ? C25 C251 H251a . . . 111(3) ? C25 C251 H251b . . . 111(3) ? C25 C251 H251c . . . 111(3) ? H251a C251 H251b . . . 107(3) ? H251a C251 H251c . . . 108(3) ? H251b C251 H251c . . . 108(3) ? Tl2 N31 Tl3 . . . 94.0(7) ? Tl2 N31 N32 . . . 127.7(16) ? Tl2 N31 C35 . . . 123.1(17) ? Tl3 N31 N32 . . . 65.2(11) ? Tl3 N31 C35 . . . 125.2(15) ? N32 N31 C35 . . . 107(2) ? Tl1 N32 Tl3 . . . 99.9(7) ? Tl1 N32 N31 . . . 120.9(15) ? Tl1 N32 C33 . . . 114.8(15) ? Tl3 N32 N31 . . . 87.6(12) ? Tl3 N32 C33 . . . 122.6(14) ? N31 N32 C33 . . . 109(2) ? N32 C33 C331 . . . 123(2) ? N32 C33 C34 . . . 108(2) ? C331 C33 C34 . . . 129(3) ? C33 C331 C332 . . . 121(3) ? C33 C331 C336 . . . 122(3) ? C332 C331 C336 . . . 117(3) ? C331 C332 C333 . . . 122(3) ? C331 C332 H332 . . . 120(3) ? C333 C332 H332 . . . 119(3) ? C332 C333 C334 . . . 117(3) ? C332 C333 H333 . . . 122(3) ? C334 C333 H333 . . . 121(3) ? C333 C334 C335 . . . 121(3) ? C333 C334 H334 . . . 120(3) ? C335 C334 H334 . . . 119(3) ? C334 C335 C336 . . . 120(3) ? C334 C335 H335 . . . 121(3) ? C336 C335 H335 . . . 119(3) ? C331 C336 C335 . . . 123(3) ? C331 C336 H336 . . . 118(3) ? C335 C336 H336 . . . 119(3) ? C33 C34 C35 . . . 105(2) ? C33 C34 H34 . . . 126(3) ? C35 C34 H34 . . . 129(3) ? N31 C35 C34 . . . 111(2) ? N31 C35 C351 . . . 121(2) ? C34 C35 C351 . . . 128(3) ? C35 C351 H351a . . . 111(3) ? C35 C351 H351b . . . 111(2) ? C35 C351 H351c . . . 111(2) ? H351a C351 H351b . . . 108(3) ? H351a C351 H351c . . . 108(3) ? H351b C351 H351c . . . 108(3) ? C0 Cl1 Cl1 . . '3 666' 86(5) ? C0 Cl1 Cl2 . . '3 666' 156(6) ? Cl1 Cl1 Cl2 '3 666' . '3 666' 73(4) ? C0 Cl2 Cl1 . . '3 666' 108(6) ? Cl1 C0 Cl2 . . . 89(7) ? Cl1 C0 H0a . . . 114(*) ? Cl1 C0 H0b . . . 118(9) ? Cl2 C0 H0a . . . 117(9) ? Cl2 C0 H0b . . . 121(11) ? H0a C0 H0b . . . 100(11) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Tl1 Tl2 4.4103(16) . . ? Tl1 Tl3 4.6704(16) . '1 655' ? Tl1 Tl4 4.4041(16) . . ? Tl1 O0 4.162(18) . . ? Tl1 O0 3.995(19) . '1 655' ? Tl1 C13 3.52(3) . . ? Tl1 C132 4.18(3) . . ? Tl1 C14 4.09(3) . . ? Tl1 C15 3.80(3) . . ? Tl1 N21 3.47(2) . . ? Tl1 C23 3.30(2) . . ? Tl1 C231 3.50(2) . . ? Tl1 C232 3.47(3) . . ? Tl1 N31 3.54(2) . . ? Tl1 C33 3.43(3) . . ? Tl1 C331 3.64(3) . . ? Tl1 C332 3.32(3) . . ? Tl1 C351 3.90(3) . '1 655' ? Tl1 H132 3.4304(13) . . ? Tl1 H232 3.2221(11) . . ? Tl1 H332 2.8616(11) . . ? Tl1 H351c 3.0142(11) . '1 655' ? Tl1 H0 3.3004(11) . '1 655' ? Tl2 C23 3.60(2) . . ? Tl2 C232 4.11(3) . . ? Tl2 C236 4.02(2) . '1 455' ? Tl2 C25 3.89(3) . . ? Tl2 N32 3.59(2) . . ? Tl2 C35 3.50(3) . . ? Tl2 C351 3.68(3) . . ? Tl2 H232 3.3347(11) . . ? Tl2 H351b 3.3870(13) . . ? Tl2 H351c 3.6039(13) . . ? Tl2 H0 2.6568(11) . . ? Tl3 Tl4 4.2791(18) . . ? Tl3 N12 3.55(2) . . ? Tl3 C14 3.99(3) . '1 455' ? Tl3 C15 3.67(3) . . ? Tl3 C151 3.92(3) . . ? Tl3 C24 3.91(3) . '4 454' ? Tl3 C33 3.64(2) . . ? Tl3 C332 4.18(3) . . ? Tl3 C333 4.03(3) . '1 455' ? Tl3 C35 3.93(3) . . ? Tl3 Cl2 4.35(7) . . ? Tl3 H24 3.1027(12) . '4 454' ? Tl3 H332 3.4303(12) . . ? Tl3 H333 3.4030(12) . '1 455' ? Tl3 H151c 3.6651(12) . . ? Tl3 H251a 3.3605(11) . '4 454' ? Tl3 H0 2.7611(12) . . ? Tl4 N11 3.53(2) . . ? Tl4 C13 3.45(3) . . ? Tl4 C131 3.62(3) . . ? Tl4 C131 3.97(3) . '1 455' ? Tl4 C132 3.47(3) . . ? Tl4 C132 3.95(3) . '1 455' ? Tl4 C133 3.83(3) . '1 455' ? Tl4 C134 3.64(3) . '1 455' ? Tl4 C135 3.58(3) . '1 455' ? Tl4 C136 3.71(3) . '1 455' ? Tl4 N22 3.58(2) . . ? Tl4 C235 3.91(3) . '4 454' ? Tl4 C236 3.82(2) . '4 454' ? Tl4 C25 3.58(2) . . ? Tl4 C251 3.71(3) . . ? Tl4 H132 3.1555(11) . . ? Tl4 H235 3.6694(12) . '4 454' ? Tl4 H236 3.5994(12) . '4 454' ? Tl4 H335 3.6435(13) . '2 646' ? Tl4 H251b 3.5128(11) . . ? Tl4 H251c 3.4859(12) . . ? Tl4 H0 2.9824(12) . . ? O0 N11 3.37(3) . . ? O0 N12 3.32(3) . . ? O0 C13 3.58(3) . '1 455' ? O0 C131 3.41(3) . '1 455' ? O0 C132 3.56(3) . '1 455' ? O0 N21 3.34(3) . . ? O0 N22 3.52(2) . . ? O0 N31 3.22(3) . . ? O0 N32 3.57(3) . . ? N11 C13 2.19(4) . . ? N11 C14 2.19(4) . . ? N11 C151 2.51(4) . . ? N12 C131 2.45(3) . . ? N12 C132 3.00(3) . . ? N12 C14 2.24(3) . . ? N12 C15 2.19(3) . . ? C13 C132 2.53(4) . . ? C13 C136 2.49(4) . . ? C13 C15 2.18(4) . . ? C13 H14 2.16(3) . . ? C131 C133 2.44(4) . . ? C131 C134 2.81(4) . . ? C131 C135 2.44(4) . . ? C131 C14 2.62(4) . . ? C131 H132 2.05(3) . . ? C131 H136 2.05(3) . . ? C132 C134 2.40(4) . . ? C132 C135 2.78(4) . . ? C132 C136 2.38(4) . . ? C132 H133 2.03(3) . . ? C133 C135 2.45(4) . . ? C133 C136 2.76(4) . . ? C133 H132 2.02(3) . . ? C133 H134 2.11(3) . . ? C134 C136 2.36(4) . . ? C134 H133 2.12(3) . . ? C134 H135 2.07(3) . . ? C135 H134 2.04(3) . . ? C135 H136 2.01(3) . . ? C136 H135 2.03(3) . . ? C14 C151 2.55(4) . . ? C15 H14 2.05(3) . . ? C15 H151a 2.09(3) . . ? C15 H151b 2.08(3) . . ? C15 H151c 2.08(3) . . ? N21 C23 2.23(3) . . ? N21 C24 2.22(3) . . ? N21 C251 2.39(4) . . ? N22 C231 2.45(3) . . ? N22 C232 2.96(3) . . ? N22 C24 2.25(3) . . ? N22 C25 2.21(3) . . ? C23 C232 2.50(4) . . ? C23 C236 2.48(3) . . ? C23 C25 2.24(4) . . ? C23 H24 2.15(2) . . ? C231 C233 2.41(4) . . ? C231 C234 2.83(4) . . ? C231 C235 2.40(3) . . ? C231 C24 2.61(4) . . ? C231 H232 2.03(2) . . ? C231 H236 2.04(2) . . ? C232 C234 2.41(4) . . ? C232 C235 2.71(3) . . ? C232 C236 2.35(3) . . ? C232 H233 2.02(3) . . ? C233 C235 2.35(4) . . ? C233 C236 2.71(4) . . ? C233 H232 2.02(2) . . ? C233 H234 2.09(2) . . ? C234 C236 2.37(4) . . ? C234 H233 2.06(3) . . ? C234 H235 2.00(3) . . ? C235 H234 2.07(3) . . ? C235 H236 2.00(3) . . ? C236 H235 2.01(2) . . ? C24 C251 2.58(4) . . ? C25 H24 2.13(2) . . ? C25 H251a 2.00(3) . . ? C25 H251b 2.00(3) . . ? C25 H251c 1.99(3) . . ? N31 C33 2.22(3) . . ? N31 C34 2.24(4) . . ? N31 C351 2.52(4) . . ? N32 C331 2.47(4) . . ? N32 C332 2.94(4) . . ? N32 C34 2.24(4) . . ? N32 C35 2.18(4) . . ? C33 C332 2.49(4) . . ? C33 C336 2.47(4) . . ? C33 C35 2.21(4) . . ? C33 H34 2.15(3) . . ? C331 C333 2.46(4) . . ? C331 C334 2.79(5) . . ? C331 C335 2.39(4) . . ? C331 C34 2.59(4) . . ? C331 H332 2.07(3) . . ? C331 H336 2.02(3) . . ? C332 C334 2.41(5) . . ? C332 C335 2.75(5) . . ? C332 C336 2.38(4) . . ? C332 Cl1 3.66(8) . . ? C332 H333 2.08(3) . . ? C333 C335 2.43(4) . . ? C333 C336 2.78(4) . . ? C333 Cl1 3.54(7) . . ? C333 Cl2 3.91(8) . '1 655' ? C333 H332 2.06(3) . . ? C333 H334 2.08(3) . . ? C334 C336 2.36(5) . . ? C334 Cl1 3.78(7) . . ? C334 Cl2 3.91(8) . '1 655' ? C334 H333 2.09(4) . . ? C334 H335 2.06(4) . . ? C335 H334 2.05(3) . . ? C335 H336 2.02(3) . . ? C336 H335 2.01(3) . . ? C34 C351 2.61(4) . . ? C35 H34 2.12(3) . . ? C35 H351a 2.09(3) . . ? C35 H351b 2.08(3) . . ? C35 H351c 2.09(3) . . ? Cl1 Cl2 2.33(9) . . ? Cl1 C0 2.67(14) . '3 666' ? Cl1 H0a 2.40(7) . . ? Cl1 H0a 3.26(8) . '3 666' ? Cl1 H0b 2.41(7) . . ? Cl2 Cl2 3.56(10) . '3 666' ? Cl2 Cl2 4.32(9) . '3 566' ? Cl2 C0 3.48(14) . '3 666' ? Cl2 H333 3.26(7) . '1 455' ? Cl2 H334 3.24(7) . '1 455' ? Cl2 H251a 3.38(7) . '4 454' ? Cl2 H0a 2.21(7) . . ? Cl2 H0b 2.21(6) . . ? H151a H151b 1.55133(16) . . ? H151a H151c 1.5514(2) . . ? H151b H151c 1.55134(16) . . ? H251a H251b 1.5512(3) . . ? H251a H251c 1.55128(16) . . ? H251b H251c 1.55130(18) . . ? H351a H351b 1.5514(2) . . ? H351a H351c 1.5514(2) . . ? H351b H351c 1.55130(19) . . ? H0a H0b 1.55137(18) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2412 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 31 _reflns_limit_l_min -21 _reflns_limit_l_max 21 _reflns_number_observed ? _reflns_d_resolution_high .847 _reflns_d_resolution_low 14.799 _diffrn_reflns_av_sigmaI/netI .085 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .094 _refine_ls_wR_factor_all .09 _refine_ls_goodness_of_fit_all 1.782 _refine_ls_shift/su_mean .001 #===END