# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Michael Hill' _publ_contact_author_address ; Department of Chemistry Imperial College London South Kensington London SW7 2AZ UNITED KINGDOM ; _publ_contact_author_email MIKE.HILL@IMPERIAL.AC.UK _publ_section_title ; Aggregation of thallium(I) beta-diketiminates ; _publ_requested_category FM loop_ _publ_author_name 'Michael Hill' 'Peter B. Hitchcock' 'Ruti Pongtavornpinyo' data_(1)-oct104 _database_code_depnum_ccdc_archive 'CCDC 609883' _audit_creation_date 2004-09-30T17:03:28-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C92 H114 N8 O11 Tl8, 2(C6 H14)' _chemical_formula_sum 'C104 H142 N8 O11 Tl8' _chemical_formula_weight 3315.22 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/n _symmetry_space_group_name_Hall '-P 2yac' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 12.4127(3) _cell_length_b 15.1224(3) _cell_length_c 29.4433(7) _cell_angle_alpha 90 _cell_angle_beta 95.743(1) _cell_angle_gamma 90 _cell_volume 5499.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 69437 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 2.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3116 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.1 -1 0 0 0.1 0 0 1 0.005 0 0 -1 0.005 0 1 0 0.1 0 -1 0 0.1 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 11.733 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; (see. N.W. Alcock (1970). Cryst. Computing, p271) ; _exptl_absorpt_correction_T_min 0.1777 _exptl_absorpt_correction_T_max 0.8889 _exptl_absorpt_correction_T_ave 0.7991 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.713019E-1 _diffrn_orient_matrix_ub_12 0.5446E-3 _diffrn_orient_matrix_ub_13 0.190991E-1 _diffrn_orient_matrix_ub_21 -0.382836E-1 _diffrn_orient_matrix_ub_22 -0.33471E-2 _diffrn_orient_matrix_ub_23 0.282629E-1 _diffrn_orient_matrix_ub_31 0.25283E-2 _diffrn_orient_matrix_ub_32 -0.660401E-1 _diffrn_orient_matrix_ub_33 -0.1275E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_unetI/netI 0.0616 _diffrn_reflns_number 29498 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _reflns_number_total 9534 _reflns_number_gt 6970 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; I think that O5 is a hydroxyl ligand but it was not possible to locate the hydrogen atom. SADI restraints were applied to the poorly defined hexane solvate molecule. Also, the C6S atoms became prolate and was finally included as isotropic. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+35.5270P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 9534 _refine_ls_number_parameters 598 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.05 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.182 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.178 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 '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' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tl1 Tl 0.74335(3) 0.23590(2) 0.690099(13) 0.03134(11) Uani 1 1 d . . . Tl2 Tl 1.01844(3) 0.13880(3) 0.776474(15) 0.04066(12) Uani 1 1 d . . . Tl3 Tl 0.56626(3) 0.38566(2) 0.747325(15) 0.04122(12) Uani 1 1 d . . . Tl4 Tl 0.77392(3) 0.24432(3) 0.565756(14) 0.04029(12) Uani 1 1 d . . . O1 O 0.5649(5) 0.2969(4) 0.6779(2) 0.0357(16) Uani 1 1 d . . . O2 O 0.6942(5) 0.3198(4) 0.6289(2) 0.0313(15) Uani 1 1 d . . . O3 O 0.8378(5) 0.1733(4) 0.6381(2) 0.0342(16) Uani 1 1 d . . . O4 O 0.9312(5) 0.2095(4) 0.7071(2) 0.0310(15) Uani 1 1 d . . . O5 O 0.6705(5) 0.1131(4) 0.7104(2) 0.0414(17) Uani 1 1 d . . . O6 O 0.75 0.3196(5) 0.75 0.035(2) Uani 1 2 d S . . N1 N 0.5490(6) 0.4756(5) 0.6669(3) 0.035(2) Uani 1 1 d . . . N2 N 0.5465(6) 0.2343(5) 0.5702(3) 0.0337(19) Uani 1 1 d . . . N3 N 0.9841(6) 0.2783(5) 0.6038(3) 0.036(2) Uani 1 1 d . . . N4 N 1.0072(6) 0.0405(5) 0.6992(3) 0.0308(19) Uani 1 1 d . . . C1 C 0.5657(7) 0.4328(6) 0.6322(4) 0.038(3) Uani 1 1 d . . . C2 C 0.5846(7) 0.3310(6) 0.6353(3) 0.031(2) Uani 1 1 d . . . C3 C 0.5070(7) 0.2836(6) 0.5995(4) 0.037(2) Uani 1 1 d . . . C4 C 0.5742(9) 0.4707(6) 0.5852(4) 0.049(3) Uani 1 1 d . . . H4A H 0.5054 0.4985 0.574 0.073 Uiso 1 1 calc R . . H4B H 0.5908 0.4232 0.5644 0.073 Uiso 1 1 calc R . . H4C H 0.6321 0.515 0.5868 0.073 Uiso 1 1 calc R . . C5 C 0.3892(8) 0.2959(8) 0.6044(4) 0.057(3) Uani 1 1 d . . . H5A H 0.3527 0.3191 0.5759 0.086 Uiso 1 1 calc R . . H5B H 0.3806 0.3377 0.6292 0.086 Uiso 1 1 calc R . . H5C H 0.3571 0.2389 0.6115 0.086 Uiso 1 1 calc R . . C6 C 0.5395(8) 0.5702(6) 0.6653(3) 0.037(2) Uani 1 1 d . . . C7 C 0.6314(9) 0.6211(7) 0.6772(4) 0.050(3) Uani 1 1 d . . . C8 C 0.6175(10) 0.7127(7) 0.6784(5) 0.060(3) Uani 1 1 d . . . H8 H 0.6793 0.7484 0.6868 0.072 Uiso 1 1 calc R . . C9 C 0.5203(10) 0.7538(7) 0.6683(4) 0.051(3) Uani 1 1 d . . . C10 C 0.4315(10) 0.7006(7) 0.6571(4) 0.054(3) Uani 1 1 d . . . H10 H 0.3629 0.7278 0.65 0.064 Uiso 1 1 calc R . . C11 C 0.4376(8) 0.6085(7) 0.6557(4) 0.049(3) Uani 1 1 d . . . C12 C 0.7401(9) 0.5776(8) 0.6869(6) 0.092(5) Uani 1 1 d . . . H12A H 0.7363 0.5326 0.7106 0.137 Uiso 1 1 calc R . . H12B H 0.7942 0.6222 0.6975 0.137 Uiso 1 1 calc R . . H12C H 0.7608 0.5498 0.659 0.137 Uiso 1 1 calc R . . C13 C 0.5096(11) 0.8529(7) 0.6695(4) 0.065(4) Uani 1 1 d . . . H13A H 0.4339 0.8695 0.6611 0.097 Uiso 0.5 1 calc PR . . H13B H 0.5552 0.8793 0.6478 0.097 Uiso 0.5 1 calc PR . . H13C H 0.5327 0.8744 0.7003 0.097 Uiso 0.5 1 calc PR . . H13D H 0.5806 0.8793 0.6784 0.097 Uiso 0.5 1 calc PR . . H13E H 0.4593 0.8695 0.6917 0.097 Uiso 0.5 1 calc PR . . H13F H 0.4818 0.8744 0.6391 0.097 Uiso 0.5 1 calc PR . . C14 C 0.3409(10) 0.5512(8) 0.6451(6) 0.085(5) Uani 1 1 d . . . H14A H 0.3379 0.5312 0.6133 0.128 Uiso 1 1 calc R . . H14B H 0.2753 0.5849 0.6494 0.128 Uiso 1 1 calc R . . H14C H 0.3458 0.4998 0.6655 0.128 Uiso 1 1 calc R . . C15 C 0.4790(7) 0.1854(6) 0.5369(4) 0.036(2) Uani 1 1 d . . . C16 C 0.4391(10) 0.1041(7) 0.5488(4) 0.056(3) Uani 1 1 d . . . C17 C 0.3809(11) 0.0543(8) 0.5150(5) 0.075(4) Uani 1 1 d . . . H17 H 0.3531 -0.0016 0.5229 0.09 Uiso 1 1 calc R . . C18 C 0.3619(11) 0.0831(8) 0.4703(5) 0.070(4) Uani 1 1 d . . . C19 C 0.4033(9) 0.1640(8) 0.4604(4) 0.060(3) Uani 1 1 d . . . H19 H 0.3906 0.1855 0.43 0.072 Uiso 1 1 calc R . . C20 C 0.4627(9) 0.2160(7) 0.4925(4) 0.046(3) Uani 1 1 d . . . C21 C 0.4528(12) 0.0702(7) 0.5970(5) 0.081(4) Uani 1 1 d . . . H21A H 0.5289 0.0755 0.6092 0.122 Uiso 1 1 calc R . . H21B H 0.4307 0.0081 0.5974 0.122 Uiso 1 1 calc R . . H21C H 0.4077 0.1051 0.6158 0.122 Uiso 1 1 calc R . . C22 C 0.2971(14) 0.0299(10) 0.4345(6) 0.112(6) Uani 1 1 d . . . H22A H 0.2737 -0.0253 0.4479 0.167 Uiso 0.5 1 calc PR . . H22B H 0.3417 0.0162 0.4098 0.167 Uiso 0.5 1 calc PR . . H22C H 0.2335 0.0639 0.4223 0.167 Uiso 0.5 1 calc PR . . H22D H 0.2923 0.0619 0.4054 0.167 Uiso 0.5 1 calc PR . . H22E H 0.2242 0.0204 0.4436 0.167 Uiso 0.5 1 calc PR . . H22F H 0.3324 -0.0273 0.431 0.167 Uiso 0.5 1 calc PR . . C23 C 0.5060(11) 0.3064(8) 0.4799(4) 0.074(4) Uani 1 1 d . . . H23A H 0.4708 0.3527 0.4964 0.11 Uiso 1 1 calc R . . H23B H 0.4907 0.3159 0.447 0.11 Uiso 1 1 calc R . . H23C H 0.5844 0.3085 0.4883 0.11 Uiso 1 1 calc R . . C24 C 1.0183(7) 0.2396(6) 0.6407(4) 0.031(2) Uani 1 1 d . . . C25 C 0.9398(7) 0.1782(6) 0.6633(4) 0.033(2) Uani 1 1 d . . . C26 C 0.9847(7) 0.0817(6) 0.6623(3) 0.030(2) Uani 1 1 d . . . C27 C 1.1287(7) 0.2516(7) 0.6655(4) 0.046(3) Uani 1 1 d . . . H27A H 1.1678 0.2975 0.6503 0.068 Uiso 1 1 calc R . . H27B H 1.1688 0.1958 0.6654 0.068 Uiso 1 1 calc R . . H27C H 1.1217 0.2694 0.6971 0.068 Uiso 1 1 calc R . . C28 C 0.9890(9) 0.0433(7) 0.6145(4) 0.047(3) Uani 1 1 d . . . H28A H 1.0642 0.0292 0.6098 0.071 Uiso 1 1 calc R . . H28B H 0.9605 0.0867 0.5917 0.071 Uiso 1 1 calc R . . H28C H 0.9452 -0.0106 0.6113 0.071 Uiso 1 1 calc R . . C29 C 1.0498(7) 0.3389(6) 0.5812(4) 0.039(3) Uani 1 1 d . . . C30 C 1.1179(8) 0.3078(7) 0.5502(4) 0.047(3) Uani 1 1 d . . . C31 C 1.1724(8) 0.3720(8) 0.5261(4) 0.056(3) Uani 1 1 d . . . H31 H 1.2206 0.3524 0.5051 0.067 Uiso 1 1 calc R . . C32 C 1.1590(9) 0.4612(8) 0.5316(4) 0.053(3) Uani 1 1 d . . . C33 C 1.0917(9) 0.4881(7) 0.5625(4) 0.056(3) Uani 1 1 d . . . H33 H 1.0831 0.5497 0.5671 0.067 Uiso 1 1 calc R . . C34 C 1.0342(8) 0.4291(7) 0.5880(4) 0.049(3) Uani 1 1 d . . . C35 C 1.1302(10) 0.2101(7) 0.5423(4) 0.063(4) Uani 1 1 d . . . H35A H 1.165 0.1824 0.5701 0.094 Uiso 1 1 calc R . . H35B H 1.175 0.2007 0.5171 0.094 Uiso 1 1 calc R . . H35C H 1.0587 0.1836 0.5345 0.094 Uiso 1 1 calc R . . C36 C 1.2192(11) 0.5267(9) 0.5053(5) 0.079(4) Uani 1 1 d . . . H36A H 1.1993 0.5869 0.5136 0.118 Uiso 0.5 1 calc PR . . H36B H 1.2003 0.5177 0.4725 0.118 Uiso 0.5 1 calc PR . . H36C H 1.2973 0.5183 0.5126 0.118 Uiso 0.5 1 calc PR . . H36D H 1.2653 0.495 0.4856 0.118 Uiso 0.5 1 calc PR . . H36E H 1.2643 0.5643 0.5266 0.118 Uiso 0.5 1 calc PR . . H36F H 1.1673 0.5636 0.4865 0.118 Uiso 0.5 1 calc PR . . C37 C 0.9571(10) 0.4623(7) 0.6201(5) 0.070(4) Uani 1 1 d . . . H37A H 0.887 0.4329 0.6135 0.105 Uiso 1 1 calc R . . H37B H 0.9478 0.5263 0.6162 0.105 Uiso 1 1 calc R . . H37C H 0.9862 0.4495 0.6516 0.105 Uiso 1 1 calc R . . C38 C 1.0326(8) -0.0518(6) 0.6987(3) 0.035(2) Uani 1 1 d . . . C39 C 1.1398(8) -0.0782(7) 0.6974(4) 0.044(3) Uani 1 1 d . . . C40 C 1.1621(9) -0.1698(7) 0.7016(4) 0.057(3) Uani 1 1 d . . . H40 H 1.2343 -0.1898 0.7004 0.068 Uiso 1 1 calc R . . C41 C 1.0835(11) -0.2301(7) 0.7072(4) 0.054(3) Uani 1 1 d . . . C42 C 0.9775(10) -0.2018(6) 0.7075(4) 0.049(3) Uani 1 1 d . . . H42 H 0.9219 -0.2441 0.7101 0.059 Uiso 1 1 calc R . . C43 C 0.9510(8) -0.1124(6) 0.7040(4) 0.040(3) Uani 1 1 d . . . C44 C 1.2291(9) -0.0133(8) 0.6913(5) 0.069(4) Uani 1 1 d . . . H44A H 1.2225 0.0078 0.6596 0.103 Uiso 1 1 calc R . . H44B H 1.2994 -0.0423 0.6982 0.103 Uiso 1 1 calc R . . H44C H 1.2236 0.037 0.7119 0.103 Uiso 1 1 calc R . . C45 C 1.1098(12) -0.3289(7) 0.7125(5) 0.078(4) Uani 1 1 d . . . H45A H 1.0432 -0.3619 0.7161 0.117 Uiso 0.5 1 calc PR . . H45B H 1.1617 -0.338 0.7394 0.117 Uiso 0.5 1 calc PR . . H45C H 1.1412 -0.35 0.6852 0.117 Uiso 0.5 1 calc PR . . H45D H 1.1875 -0.338 0.711 0.117 Uiso 0.5 1 calc PR . . H45E H 1.0691 -0.362 0.6878 0.117 Uiso 0.5 1 calc PR . . H45F H 1.0896 -0.3499 0.7419 0.117 Uiso 0.5 1 calc PR . . C46 C 0.8369(9) -0.0795(7) 0.7043(5) 0.067(4) Uani 1 1 d . . . H46A H 0.8337 -0.0365 0.729 0.1 Uiso 1 1 calc R . . H46B H 0.7889 -0.1294 0.7091 0.1 Uiso 1 1 calc R . . H46C H 0.8137 -0.0512 0.675 0.1 Uiso 1 1 calc R . . C1S C 0.8353(14) -0.2655(14) 0.5936(7) 0.142(8) Uani 1 1 d D . . H1S1 H 0.7973 -0.3221 0.5951 0.213 Uiso 1 1 calc R . . H1S2 H 0.7993 -0.2293 0.569 0.213 Uiso 1 1 calc R . . H1S3 H 0.8344 -0.2343 0.6228 0.213 Uiso 1 1 calc R . . C2S C 0.9525(13) -0.2825(10) 0.5843(6) 0.103(6) Uani 1 1 d D . . H2S1 H 0.9873 -0.3202 0.6091 0.123 Uiso 1 1 calc R . . H2S2 H 0.9521 -0.316 0.5554 0.123 Uiso 1 1 calc R . . C3S C 1.0198(13) -0.2009(9) 0.5809(6) 0.095(5) Uani 1 1 d D . . H3S1 H 1.0276 -0.1709 0.6109 0.114 Uiso 1 1 calc R . . H3S2 H 0.9812 -0.16 0.5586 0.114 Uiso 1 1 calc R . . C4S C 1.1312(14) -0.2188(11) 0.5665(6) 0.110(6) Uani 1 1 d D . . H4S1 H 1.1703 -0.2583 0.5894 0.132 Uiso 1 1 calc R . . H4S2 H 1.1231 -0.2508 0.537 0.132 Uiso 1 1 calc R . . C5S C 1.1993(18) -0.1378(13) 0.5613(6) 0.139(8) Uani 1 1 d D . . H5S1 H 1.2683 -0.1551 0.5496 0.167 Uiso 1 1 calc R . . H5S2 H 1.2166 -0.1095 0.5915 0.167 Uiso 1 1 calc R . . C6S C 1.139(2) -0.071(2) 0.5281(11) 0.255(16) Uiso 1 1 d D . . H6S1 H 1.1836 -0.0186 0.5256 0.383 Uiso 1 1 calc R . . H6S2 H 1.0703 -0.0544 0.5397 0.383 Uiso 1 1 calc R . . H6S3 H 1.1236 -0.0988 0.498 0.383 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl1 0.0349(2) 0.03098(19) 0.0294(2) 0.00122(16) 0.00969(17) 0.00349(16) Tl2 0.0386(2) 0.0434(2) 0.0399(3) -0.00264(19) 0.00349(18) 0.00837(18) Tl3 0.0494(2) 0.0348(2) 0.0421(3) -0.00045(18) 0.0178(2) 0.00760(18) Tl4 0.0412(2) 0.0510(2) 0.0299(3) 0.00031(19) 0.00943(18) 0.00069(19) O1 0.040(4) 0.028(3) 0.040(5) 0.003(3) 0.010(3) 0.003(3) O2 0.033(3) 0.031(3) 0.030(4) 0.001(3) 0.005(3) 0.001(3) O3 0.030(4) 0.037(4) 0.037(4) -0.001(3) 0.009(3) -0.002(3) O4 0.034(3) 0.029(3) 0.032(4) -0.003(3) 0.009(3) 0.002(3) O5 0.052(4) 0.029(3) 0.044(5) -0.003(3) 0.015(3) -0.008(3) O6 0.047(5) 0.027(5) 0.031(6) 0 0.011(5) 0 N1 0.044(5) 0.028(4) 0.036(6) -0.005(4) 0.012(4) 0.001(4) N2 0.045(5) 0.030(4) 0.025(5) 0.004(4) -0.002(4) 0.001(4) N3 0.034(4) 0.036(4) 0.041(6) 0.002(4) 0.014(4) -0.008(4) N4 0.038(4) 0.027(4) 0.028(5) -0.002(4) 0.008(4) 0.000(4) C1 0.028(5) 0.030(5) 0.056(8) 0.017(5) -0.001(5) -0.001(4) C2 0.029(5) 0.034(5) 0.030(6) 0.003(4) 0.002(4) 0.006(4) C3 0.032(5) 0.035(5) 0.044(7) 0.013(5) -0.002(5) 0.002(5) C4 0.079(8) 0.031(5) 0.038(7) 0.006(5) 0.015(6) 0.006(5) C5 0.036(6) 0.065(7) 0.069(10) 0.000(7) 0.000(6) 0.000(6) C6 0.055(7) 0.025(5) 0.034(7) 0.000(4) 0.012(5) 0.001(5) C7 0.051(7) 0.036(6) 0.062(9) -0.004(5) 0.011(6) 0.008(5) C8 0.053(7) 0.041(6) 0.088(11) -0.015(6) 0.015(7) -0.011(6) C9 0.076(8) 0.044(6) 0.038(7) -0.006(5) 0.026(6) 0.007(7) C10 0.063(8) 0.039(6) 0.060(9) -0.004(6) 0.012(6) 0.030(6) C11 0.041(6) 0.054(7) 0.054(8) -0.002(6) 0.007(6) 0.013(6) C12 0.052(8) 0.040(7) 0.180(18) -0.003(8) -0.003(9) 0.002(6) C13 0.092(9) 0.035(6) 0.070(10) 0.001(6) 0.023(8) 0.013(6) C14 0.054(8) 0.068(9) 0.132(15) -0.027(9) 0.002(8) 0.021(7) C15 0.030(5) 0.041(6) 0.036(7) -0.011(5) 0.005(5) -0.007(5) C16 0.076(8) 0.039(6) 0.047(8) 0.004(6) -0.014(6) -0.015(6) C17 0.101(11) 0.048(7) 0.072(11) 0.002(7) -0.012(9) -0.024(7) C18 0.088(10) 0.049(7) 0.067(11) -0.007(7) -0.014(8) -0.023(7) C19 0.072(8) 0.073(8) 0.031(8) -0.004(6) -0.014(6) -0.004(7) C20 0.057(7) 0.050(6) 0.029(7) 0.009(5) -0.003(6) 0.000(5) C21 0.127(12) 0.043(7) 0.073(11) 0.021(7) 0.001(9) -0.029(8) C22 0.139(15) 0.086(11) 0.101(15) -0.023(10) -0.029(11) -0.040(11) C23 0.108(11) 0.060(8) 0.049(9) 0.019(7) -0.007(8) -0.027(8) C24 0.030(5) 0.026(5) 0.039(7) 0.001(5) 0.012(4) 0.006(4) C25 0.032(5) 0.026(5) 0.043(7) 0.000(4) 0.017(5) 0.001(4) C26 0.031(5) 0.029(5) 0.032(7) -0.001(4) 0.012(5) -0.005(4) C27 0.032(5) 0.053(7) 0.051(8) 0.010(5) 0.001(5) -0.008(5) C28 0.054(7) 0.042(6) 0.049(8) 0.000(5) 0.019(6) 0.008(5) C29 0.026(5) 0.042(6) 0.050(8) 0.009(5) 0.002(5) -0.006(5) C30 0.039(6) 0.053(7) 0.052(8) 0.003(6) 0.014(6) 0.009(5) C31 0.041(6) 0.074(9) 0.054(9) 0.006(7) 0.016(6) -0.003(6) C32 0.046(6) 0.062(8) 0.053(9) 0.027(6) 0.013(6) -0.010(6) C33 0.076(8) 0.035(6) 0.059(9) 0.009(6) 0.018(7) -0.008(6) C34 0.045(6) 0.047(6) 0.057(9) 0.015(6) 0.014(6) -0.004(5) C35 0.067(8) 0.063(8) 0.064(9) -0.002(7) 0.033(7) 0.011(7) C36 0.093(10) 0.079(9) 0.071(11) 0.021(8) 0.037(8) -0.013(8) C37 0.092(10) 0.035(6) 0.089(11) 0.011(6) 0.040(8) 0.004(6) C38 0.040(6) 0.036(5) 0.029(6) 0.002(4) 0.002(5) 0.006(5) C39 0.046(6) 0.046(6) 0.038(7) -0.009(5) -0.004(5) 0.002(5) C40 0.046(7) 0.054(7) 0.069(10) -0.013(6) 0.005(6) 0.024(6) C41 0.082(9) 0.039(6) 0.041(8) -0.006(5) 0.004(6) 0.007(7) C42 0.079(8) 0.026(5) 0.045(8) 0.002(5) 0.015(6) -0.003(6) C43 0.049(6) 0.031(5) 0.043(7) -0.007(5) 0.017(5) -0.007(5) C44 0.048(7) 0.069(8) 0.089(11) -0.001(7) 0.005(7) 0.016(7) C45 0.122(12) 0.030(6) 0.079(11) 0.000(6) -0.002(9) 0.015(7) C46 0.067(8) 0.052(7) 0.086(11) -0.009(7) 0.034(8) -0.018(6) C1S 0.117(15) 0.21(2) 0.097(17) -0.039(15) 0.001(12) 0.052(15) C2S 0.144(16) 0.084(11) 0.073(13) -0.011(9) -0.025(11) -0.003(11) C3S 0.131(14) 0.076(10) 0.077(13) -0.013(9) 0.000(11) 0.018(10) C4S 0.163(18) 0.086(11) 0.084(14) -0.027(10) 0.025(12) -0.036(12) C5S 0.20(2) 0.153(18) 0.070(14) -0.035(13) 0.023(14) -0.038(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O6 2.166(5) . ? Tl1 O5 2.175(6) . ? Tl1 O3 2.229(6) . ? Tl1 O2 2.238(6) . ? Tl1 O4 2.369(6) . ? Tl1 O1 2.394(6) . ? Tl2 O5 2.446(6) 2_656 ? Tl2 O4 2.460(6) . ? Tl3 O1 2.444(6) . ? Tl3 O6 2.484(3) . ? Tl4 O3 2.447(7) . ? Tl4 O2 2.470(6) . ? O1 C2 1.400(11) . ? O2 C2 1.403(10) . ? O3 C25 1.403(11) . ? O4 C25 1.388(11) . ? O5 Tl2 2.446(6) 2_656 ? O6 Tl1 2.166(5) 2_656 ? O6 Tl3 2.484(3) 2_656 ? N1 C1 1.244(12) . ? N1 C6 1.435(11) . ? N2 C3 1.274(12) . ? N2 C15 1.430(12) . ? N3 C24 1.268(12) . ? N3 C29 1.434(11) . ? N4 C26 1.258(11) . ? N4 C38 1.432(11) . ? C1 C4 1.511(14) . ? C1 C2 1.558(12) . ? C2 C3 1.534(14) . ? C3 C5 1.495(13) . ? C6 C7 1.392(14) . ? C6 C11 1.394(14) . ? C7 C8 1.396(14) . ? C7 C12 1.503(15) . ? C8 C9 1.364(16) . ? C9 C10 1.378(16) . ? C9 C13 1.505(14) . ? C10 C11 1.396(14) . ? C11 C14 1.488(16) . ? C15 C20 1.384(14) . ? C15 C16 1.385(14) . ? C16 C17 1.392(16) . ? C16 C21 1.502(16) . ? C17 C18 1.383(18) . ? C18 C19 1.370(16) . ? C18 C22 1.495(18) . ? C19 C20 1.383(15) . ? C20 C23 1.527(15) . ? C24 C27 1.499(13) . ? C24 C25 1.544(12) . ? C25 C26 1.565(12) . ? C26 C28 1.528(14) . ? C29 C30 1.386(14) . ? C29 C34 1.395(14) . ? C30 C31 1.414(14) . ? C30 C35 1.507(15) . ? C31 C32 1.370(15) . ? C32 C33 1.356(15) . ? C32 C36 1.502(14) . ? C33 C34 1.406(14) . ? C34 C37 1.498(14) . ? C38 C43 1.386(13) . ? C38 C39 1.394(13) . ? C39 C40 1.415(14) . ? C39 C44 1.506(15) . ? C40 C41 1.357(15) . ? C41 C42 1.383(15) . ? C41 C45 1.534(14) . ? C42 C43 1.393(13) . ? C43 C46 1.502(14) . ? C1S C2S 1.528(14) . ? C2S C3S 1.500(13) . ? C3S C4S 1.511(14) . ? C4S C5S 1.504(14) . ? C5S C6S 1.545(16) . ? 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 O6 Tl1 O5 104.9(2) . . ? O6 Tl1 O3 145.82(16) . . ? O5 Tl1 O3 95.1(2) . . ? O6 Tl1 O2 108.1(2) . . ? O5 Tl1 O2 128.2(2) . . ? O3 Tl1 O2 78.9(2) . . ? O6 Tl1 O4 88.29(15) . . ? O5 Tl1 O4 103.0(2) . . ? O3 Tl1 O4 59.9(2) . . ? O2 Tl1 O4 116.6(2) . . ? O6 Tl1 O1 81.73(17) . . ? O5 Tl1 O1 88.1(2) . . ? O3 Tl1 O1 127.1(2) . . ? O2 Tl1 O1 59.2(2) . . ? O4 Tl1 O1 166.7(2) . . ? O5 Tl2 O4 81.4(2) 2_656 . ? O1 Tl3 O6 74.65(17) . . ? O3 Tl4 O2 70.53(19) . . ? C2 O1 Tl1 92.0(5) . . ? C2 O1 Tl3 124.0(5) . . ? Tl1 O1 Tl3 99.0(2) . . ? C2 O2 Tl1 98.6(5) . . ? C2 O2 Tl4 128.7(5) . . ? Tl1 O2 Tl4 104.3(2) . . ? C25 O3 Tl1 97.1(5) . . ? C25 O3 Tl4 129.2(5) . . ? Tl1 O3 Tl4 105.3(2) . . ? C25 O4 Tl1 91.5(5) . . ? C25 O4 Tl2 123.7(5) . . ? Tl1 O4 Tl2 126.2(2) . . ? Tl1 O5 Tl2 109.8(3) . 2_656 ? Tl1 O6 Tl1 108.5(3) . 2_656 ? Tl1 O6 Tl3 102.76(4) . 2_656 ? Tl1 O6 Tl3 104.43(4) 2_656 2_656 ? Tl1 O6 Tl3 104.43(4) . . ? Tl1 O6 Tl3 102.76(4) 2_656 . ? Tl3 O6 Tl3 132.6(3) 2_656 . ? C1 N1 C6 120.7(9) . . ? C3 N2 C15 121.9(8) . . ? C24 N3 C29 122.3(8) . . ? C26 N4 C38 120.3(8) . . ? N1 C1 C4 125.9(9) . . ? N1 C1 C2 120.2(9) . . ? C4 C1 C2 113.8(9) . . ? O1 C2 O2 109.6(7) . . ? O1 C2 C3 106.8(7) . . ? O2 C2 C3 113.6(8) . . ? O1 C2 C1 112.2(8) . . ? O2 C2 C1 104.7(7) . . ? C3 C2 C1 110.0(8) . . ? N2 C3 C5 125.8(10) . . ? N2 C3 C2 118.8(8) . . ? C5 C3 C2 115.3(9) . . ? C7 C6 C11 121.7(9) . . ? C7 C6 N1 118.7(9) . . ? C11 C6 N1 119.3(9) . . ? C6 C7 C8 117.0(10) . . ? C6 C7 C12 120.3(9) . . ? C8 C7 C12 122.7(10) . . ? C9 C8 C7 123.8(11) . . ? C8 C9 C10 117.0(10) . . ? C8 C9 C13 121.8(11) . . ? C10 C9 C13 121.1(11) . . ? C9 C10 C11 123.1(10) . . ? C6 C11 C10 117.3(10) . . ? C6 C11 C14 119.8(10) . . ? C10 C11 C14 122.8(10) . . ? C20 C15 C16 120.9(10) . . ? C20 C15 N2 119.7(9) . . ? C16 C15 N2 119.1(10) . . ? C15 C16 C17 118.2(11) . . ? C15 C16 C21 122.1(10) . . ? C17 C16 C21 119.6(11) . . ? C18 C17 C16 122.5(11) . . ? C19 C18 C17 116.8(11) . . ? C19 C18 C22 121.2(14) . . ? C17 C18 C22 122.0(12) . . ? C18 C19 C20 123.3(12) . . ? C19 C20 C15 118.2(10) . . ? C19 C20 C23 121.3(11) . . ? C15 C20 C23 120.5(10) . . ? N3 C24 C27 125.0(8) . . ? N3 C24 C25 118.4(8) . . ? C27 C24 C25 116.6(9) . . ? O4 C25 O3 111.0(7) . . ? O4 C25 C24 107.8(7) . . ? O3 C25 C24 112.3(8) . . ? O4 C25 C26 113.3(8) . . ? O3 C25 C26 104.2(7) . . ? C24 C25 C26 108.2(7) . . ? N4 C26 C28 125.6(8) . . ? N4 C26 C25 119.6(8) . . ? C28 C26 C25 114.6(8) . . ? C30 C29 C34 121.9(9) . . ? C30 C29 N3 120.1(9) . . ? C34 C29 N3 117.7(9) . . ? C29 C30 C31 116.8(10) . . ? C29 C30 C35 120.8(9) . . ? C31 C30 C35 122.3(10) . . ? C32 C31 C30 123.1(10) . . ? C33 C32 C31 117.7(10) . . ? C33 C32 C36 121.3(11) . . ? C31 C32 C36 121.0(11) . . ? C32 C33 C34 123.2(10) . . ? C29 C34 C33 117.3(10) . . ? C29 C34 C37 121.7(9) . . ? C33 C34 C37 121.1(10) . . ? C43 C38 C39 121.6(9) . . ? C43 C38 N4 118.7(8) . . ? C39 C38 N4 119.5(9) . . ? C38 C39 C40 117.2(10) . . ? C38 C39 C44 122.2(9) . . ? C40 C39 C44 120.6(10) . . ? C41 C40 C39 122.1(10) . . ? C40 C41 C42 119.2(10) . . ? C40 C41 C45 121.2(11) . . ? C42 C41 C45 119.6(11) . . ? C41 C42 C43 121.2(10) . . ? C38 C43 C42 118.7(9) . . ? C38 C43 C46 118.8(9) . . ? C42 C43 C46 122.5(9) . . ? C3S C2S C1S 114.9(15) . . ? C2S C3S C4S 113.8(13) . . ? C5S C4S C3S 114.9(15) . . ? C4S C5S C6S 111(2) . . ? #===END data_(2)-jul805 _database_code_depnum_ccdc_archive 'CCDC 609884' _audit_creation_date 2005-07-06T11:04:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H26 N2, C21 H25 N2 Tl' _chemical_formula_sum 'C42 H51 N4 Tl' _chemical_formula_weight 816.24 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 22.3307(3) _cell_length_b 16.6863(3) _cell_length_c 10.2310(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3812.24(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 39211 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.27 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.3369 _exptl_absorpt_correction_T_max 0.4599 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.51409E-2 _diffrn_orient_matrix_ub_12 -0.235317E-1 _diffrn_orient_matrix_ub_13 -0.411174E-1 _diffrn_orient_matrix_ub_21 0.90171E-1 _diffrn_orient_matrix_ub_22 0.222399E-1 _diffrn_orient_matrix_ub_23 -0.47403E-2 _diffrn_orient_matrix_ub_31 0.373671E-1 _diffrn_orient_matrix_ub_32 -0.05043 _diffrn_orient_matrix_ub_33 0.170957E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_unetI/netI 0.0256 _diffrn_reflns_number 61777 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.6 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 3883 _reflns_number_gt 3069 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H atom on N2 was refined; other H atoms were in riding mode. Slightly peculiar ADPs for the atoms of the C17 to C20 ring may represent disorder which could not be modelled. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+4.6465P] 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_number_reflns 3883 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0556 _refine_ls_wR_factor_gt 0.0512 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.414 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 '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' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tl Tl 0.159384(8) 0.25 0.255485(17) 0.03497(7) Uani 1 2 d S . . N1 N 0.10443(10) 0.16057(15) 0.3949(2) 0.0284(6) Uani 1 1 d . . . N2 N 0.20882(17) 0.25 -0.0894(4) 0.0410(11) Uani 1 2 d S . . H2X H 0.226(2) 0.25 -0.018(5) 0.043(15) Uiso 1 2 d S . . N3 N 0.30537(15) 0.25 0.0545(3) 0.0326(9) Uani 1 2 d S . . C1 C 0.07501(13) 0.1740(2) 0.5054(3) 0.0287(7) Uani 1 1 d . . . C2 C 0.06459(19) 0.25 0.5594(4) 0.0287(10) Uani 1 2 d S . . H2 H 0.0481 0.25 0.645 0.034 Uiso 1 2 calc SR . . C3 C 0.05038(15) 0.1032(2) 0.5818(3) 0.0403(8) Uani 1 1 d . . . H3A H 0.0172 0.0789 0.5331 0.06 Uiso 1 1 calc R . . H3B H 0.036 0.1216 0.6671 0.06 Uiso 1 1 calc R . . H3C H 0.0821 0.0633 0.5943 0.06 Uiso 1 1 calc R . . C4 C 0.10668(15) 0.08274(19) 0.3397(3) 0.0333(8) Uani 1 1 d . . . C5 C 0.05963(17) 0.0563(2) 0.2600(3) 0.0445(9) Uani 1 1 d . . . C6 C 0.0661(2) -0.0167(3) 0.1962(4) 0.0608(12) Uani 1 1 d . . . H6 H 0.0349 -0.035 0.1406 0.073 Uiso 1 1 calc R . . C7 C 0.1165(3) -0.0630(3) 0.2113(4) 0.0692(14) Uani 1 1 d . . . H7 H 0.1197 -0.1127 0.1667 0.083 Uiso 1 1 calc R . . C8 C 0.1623(2) -0.0375(2) 0.2906(4) 0.0596(11) Uani 1 1 d . . . H8 H 0.1969 -0.0701 0.3013 0.071 Uiso 1 1 calc R . . C9 C 0.15844(16) 0.0358(2) 0.3555(3) 0.0417(8) Uani 1 1 d . . . C10 C 0.00376(16) 0.1057(3) 0.2446(4) 0.0611(11) Uani 1 1 d . . . H10A H -0.0212 0.0828 0.1752 0.092 Uiso 1 1 calc R . . H10B H 0.0147 0.1608 0.2217 0.092 Uiso 1 1 calc R . . H10C H -0.0187 0.1057 0.327 0.092 Uiso 1 1 calc R . . C11 C 0.20855(16) 0.0639(2) 0.4436(4) 0.0538(10) Uani 1 1 d . . . H11A H 0.1936 0.0691 0.5333 0.081 Uiso 1 1 calc R . . H11B H 0.2233 0.1159 0.4132 0.081 Uiso 1 1 calc R . . H11C H 0.2413 0.0247 0.4416 0.081 Uiso 1 1 calc R . . C12 C 0.24538(19) 0.25 -0.1927(4) 0.0271(10) Uani 1 2 d S . . C13 C 0.30629(18) 0.25 -0.1759(4) 0.0277(10) Uani 1 2 d S . . H13 H 0.3304 0.25 -0.2524 0.033 Uiso 1 2 calc SR . . C14 C 0.33635(19) 0.25 -0.0531(4) 0.0304(10) Uani 1 2 d S . . C15 C 0.2178(2) 0.25 -0.3261(4) 0.0449(13) Uani 1 2 d S . . H15A H 0.2027 0.1962 -0.3463 0.067 Uiso 0.5 1 calc PR . . H15B H 0.248 0.2654 -0.3909 0.067 Uiso 0.5 1 calc PR . . H15C H 0.1845 0.2884 -0.3283 0.067 Uiso 0.5 1 calc PR . . C16 C 0.40379(19) 0.25 -0.0533(5) 0.0477(14) Uani 1 2 d S . . H16A H 0.4184 0.3052 -0.0596 0.071 Uiso 0.5 1 calc PR . . H16B H 0.4184 0.2191 -0.1282 0.071 Uiso 0.5 1 calc PR . . H16C H 0.4185 0.2257 0.0278 0.071 Uiso 0.5 1 calc PR . . C17 C 0.14551(18) 0.25 -0.0873(4) 0.0316(11) Uani 1 2 d S . . C18 C 0.11623(18) 0.1771(3) -0.0803(3) 0.0517(10) Uani 1 1 d . . . C19 C 0.0543(2) 0.1802(5) -0.0668(4) 0.103(3) Uani 1 1 d . . . H19 H 0.0327 0.1313 -0.0614 0.124 Uiso 1 1 calc R . . C20 C 0.0237(3) 0.25 -0.0610(8) 0.138(6) Uani 1 2 d S . . H20 H -0.0187 0.25 -0.0529 0.166 Uiso 1 2 calc SR . . C21 C 0.1497(3) 0.0994(3) -0.0813(5) 0.105(2) Uani 1 1 d . . . H21A H 0.1745 0.0964 -0.1602 0.157 Uiso 1 1 calc R . . H21B H 0.1211 0.0548 -0.0808 0.157 Uiso 1 1 calc R . . H21C H 0.1753 0.0962 -0.0037 0.157 Uiso 1 1 calc R . . C22 C 0.33018(18) 0.25 0.1818(4) 0.0305(10) Uani 1 2 d S . . C23 C 0.33885(14) 0.1771(2) 0.2462(3) 0.0385(7) Uani 1 1 d . . . C24 C 0.35682(14) 0.1784(2) 0.3769(3) 0.0424(9) Uani 1 1 d . . . H24 H 0.3631 0.1294 0.4221 0.051 Uiso 1 1 calc R . . C25 C 0.3655(2) 0.25 0.4410(4) 0.0410(13) Uani 1 2 d S . . H25 H 0.3776 0.25 0.53 0.049 Uiso 1 2 calc SR . . C26 C 0.32773(19) 0.0991(2) 0.1764(4) 0.0575(11) Uani 1 1 d . . . H26A H 0.2853 0.0954 0.1523 0.086 Uiso 1 1 calc R . . H26B H 0.3382 0.0544 0.2342 0.086 Uiso 1 1 calc R . . H26C H 0.3524 0.0967 0.0974 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl 0.04137(11) 0.02873(10) 0.03481(10) 0 0.01572(8) 0 N1 0.0304(14) 0.0230(14) 0.0317(13) -0.0020(11) 0.0048(11) -0.0015(11) N2 0.027(2) 0.072(3) 0.024(2) 0 -0.0029(17) 0 N3 0.0236(19) 0.050(3) 0.0241(19) 0 -0.0012(15) 0 C1 0.0244(16) 0.0322(19) 0.0296(16) 0.0034(14) -0.0007(12) -0.0034(14) C2 0.026(2) 0.033(3) 0.027(2) 0 0.0067(18) 0 C3 0.047(2) 0.035(2) 0.0380(18) 0.0073(16) 0.0094(15) -0.0074(17) C4 0.045(2) 0.0237(18) 0.0313(16) 0.0024(14) 0.0109(14) -0.0053(15) C5 0.057(2) 0.041(2) 0.0354(18) 0.0042(18) 0.0058(18) -0.0183(18) C6 0.095(3) 0.048(3) 0.039(2) -0.004(2) 0.002(2) -0.036(3) C7 0.130(4) 0.028(2) 0.050(2) -0.0121(19) 0.026(3) -0.014(3) C8 0.088(3) 0.030(2) 0.061(2) -0.0047(19) 0.021(2) 0.002(2) C9 0.053(2) 0.0267(19) 0.0456(19) 0.0010(16) 0.0130(17) 0.0000(18) C10 0.052(2) 0.079(3) 0.053(2) 0.003(2) -0.0084(19) -0.017(2) C11 0.047(2) 0.041(2) 0.074(3) 0.005(2) 0.002(2) 0.0113(19) C12 0.033(2) 0.024(2) 0.024(2) 0 0.0005(18) 0 C13 0.026(2) 0.032(3) 0.025(2) 0 0.0042(17) 0 C14 0.027(2) 0.029(3) 0.035(2) 0 0.000(2) 0 C15 0.035(3) 0.069(4) 0.031(3) 0 -0.004(2) 0 C16 0.026(2) 0.077(4) 0.040(3) 0 0.002(2) 0 C17 0.025(2) 0.050(3) 0.020(2) 0 -0.0017(17) 0 C18 0.060(2) 0.064(3) 0.0315(19) -0.0078(18) 0.0057(17) -0.025(2) C19 0.068(4) 0.198(8) 0.043(3) -0.016(4) 0.011(3) -0.085(4) C20 0.020(4) 0.34(2) 0.053(4) 0 0.002(3) 0 C21 0.200(7) 0.040(3) 0.075(3) -0.012(3) 0.035(4) -0.019(4) C22 0.020(2) 0.042(3) 0.030(2) 0 0.0004(18) 0 C23 0.0353(16) 0.045(2) 0.0348(17) 0.0000(17) -0.0004(15) 0.0002(15) C24 0.0394(19) 0.055(3) 0.0327(18) 0.0094(17) -0.0028(14) 0.0060(18) C25 0.028(2) 0.069(4) 0.027(2) 0 -0.004(2) 0 C26 0.077(3) 0.046(3) 0.049(2) 0.0022(19) -0.011(2) 0.003(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Tl N1 2.401(2) 8_565 ? Tl N1 2.401(2) . ? N1 C1 1.327(4) . ? N1 C4 1.417(4) . ? N2 C12 1.336(5) . ? N2 C17 1.414(5) . ? N2 H2X 0.82(5) . ? N3 C14 1.300(5) . ? N3 C22 1.415(5) . ? C1 C2 1.402(4) . ? C1 C3 1.520(4) . ? C2 C1 1.402(4) 8_565 ? C2 H2 0.95 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 C5 1.401(5) . ? C4 C9 1.406(5) . ? C5 C6 1.389(6) . ? C5 C10 1.504(5) . ? C6 C7 1.374(6) . ? C6 H6 0.95 . ? C7 C8 1.373(6) . ? C7 H7 0.95 . ? C8 C9 1.395(5) . ? C8 H8 0.95 . ? C9 C11 1.512(5) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 C13 1.371(6) . ? C12 C15 1.497(6) . ? C13 C14 1.425(6) . ? C13 H13 0.95 . ? C14 C16 1.506(6) . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 C18 1.383(4) 8_565 ? C17 C18 1.383(4) . ? C18 C19 1.390(6) . ? C18 C21 1.496(6) . ? C19 C20 1.353(7) . ? C19 H19 0.95 . ? C20 C19 1.353(7) 8_565 ? C20 H20 0.95 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C23 1.397(4) 8_565 ? C22 C23 1.397(4) . ? C23 C24 1.396(4) . ? C23 C26 1.505(5) . ? C24 C25 1.376(4) . ? C24 H24 0.95 . ? C25 C24 1.376(4) 8_565 ? C25 H25 0.95 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Tl N1 76.84(12) 8_565 . ? C1 N1 C4 120.8(3) . . ? C1 N1 Tl 130.9(2) . . ? C4 N1 Tl 108.36(17) . . ? C12 N2 C17 128.6(4) . . ? C12 N2 H2X 114(3) . . ? C17 N2 H2X 117(3) . . ? C14 N3 C22 124.8(3) . . ? N1 C1 C2 124.8(3) . . ? N1 C1 C3 119.1(3) . . ? C2 C1 C3 116.1(3) . . ? C1 C2 C1 129.4(4) . 8_565 ? C1 C2 H2 115.3 . . ? C1 C2 H2 115.3 8_565 . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C9 120.5(3) . . ? C5 C4 N1 119.6(3) . . ? C9 C4 N1 119.6(3) . . ? C6 C5 C4 118.1(4) . . ? C6 C5 C10 121.2(4) . . ? C4 C5 C10 120.7(3) . . ? C7 C6 C5 121.7(4) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C8 C7 C6 120.2(4) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 120.4(4) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C9 C4 119.0(4) . . ? C8 C9 C11 120.7(4) . . ? C4 C9 C11 120.3(3) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C13 120.5(4) . . ? N2 C12 C15 118.0(4) . . ? C13 C12 C15 121.5(4) . . ? C12 C13 C14 125.3(4) . . ? C12 C13 H13 117.4 . . ? C14 C13 H13 117.4 . . ? N3 C14 C13 119.8(4) . . ? N3 C14 C16 122.2(4) . . ? C13 C14 C16 118.0(4) . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C18 123.2(5) 8_565 . ? C18 C17 N2 118.3(2) 8_565 . ? C18 C17 N2 118.3(2) . . ? C17 C18 C19 116.3(5) . . ? C17 C18 C21 121.7(4) . . ? C19 C18 C21 121.9(5) . . ? C20 C19 C18 122.7(6) . . ? C20 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? C19 C20 C19 118.9(7) 8_565 . ? C19 C20 H20 120.6 8_565 . ? C19 C20 H20 120.6 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C23 121.1(4) 8_565 . ? C23 C22 N3 119.2(2) 8_565 . ? C23 C22 N3 119.2(2) . . ? C24 C23 C22 118.5(3) . . ? C24 C23 C26 121.0(3) . . ? C22 C23 C26 120.4(3) . . ? C25 C24 C23 120.7(4) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C24 120.4(4) . 8_565 ? C24 C25 H25 119.8 . . ? C24 C25 H25 119.8 8_565 . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? #===END data_(3)-dec905 _database_code_depnum_ccdc_archive 'CCDC 609885' _audit_creation_date 2005-12-15T11:51:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C63 H75 N6 Tl3' _chemical_formula_sum 'C63 H75 N6 Tl3' _chemical_formula_weight 1529.4 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0548(2) _cell_length_b 12.3991(3) _cell_length_c 24.0307(5) _cell_angle_alpha 92.243(2) _cell_angle_beta 98.399(1) _cell_angle_gamma 97.355(1) _cell_volume 2934.29(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 29976 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.26 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.3742 _exptl_absorpt_correction_T_max 0.5388 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.622319E-1 _diffrn_orient_matrix_ub_12 -0.147804E-1 _diffrn_orient_matrix_ub_13 -0.367083E-1 _diffrn_orient_matrix_ub_21 0.789698E-1 _diffrn_orient_matrix_ub_22 0.160799E-1 _diffrn_orient_matrix_ub_23 -0.206904E-1 _diffrn_orient_matrix_ub_31 0.136514E-1 _diffrn_orient_matrix_ub_32 -0.784793E-1 _diffrn_orient_matrix_ub_33 0.96E-4 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_av_unetI/netI 0.0669 _diffrn_reflns_number 39677 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 26.03 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 11528 _reflns_number_gt 8721 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00050(10) _refine_ls_number_reflns 11528 _refine_ls_number_parameters 668 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.097 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.483 _refine_diff_density_min -2.109 _refine_diff_density_rms 0.192 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 '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' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tl1 Tl 0.32949(3) 0.23792(2) 0.229198(11) 0.02882(10) Uani 1 1 d . . . Tl2 Tl 0.61718(3) 0.17222(2) 0.321394(11) 0.02905(10) Uani 1 1 d . . . Tl3 Tl 0.92502(3) 0.22413(2) 0.246680(12) 0.03224(10) Uani 1 1 d . . . N1 N 0.2083(6) 0.0653(5) 0.2550(2) 0.0282(14) Uani 1 1 d . . . N2 N 0.2022(6) 0.1551(5) 0.1391(2) 0.0305(14) Uani 1 1 d . . . N3 N 0.6755(5) 0.3456(5) 0.2736(2) 0.0280(14) Uani 1 1 d . . . N4 N 0.5825(6) 0.1139(4) 0.2188(2) 0.0267(14) Uani 1 1 d . . . N5 N 1.0589(6) 0.4005(5) 0.2320(3) 0.0327(15) Uani 1 1 d . . . N6 N 1.0257(6) 0.2955(5) 0.3452(2) 0.0310(14) Uani 1 1 d . . . C1 C 0.1064(7) -0.0008(6) 0.2260(3) 0.0307(17) Uani 1 1 d . . . C2 C 0.0493(8) 0.0101(6) 0.1697(3) 0.0339(18) Uani 1 1 d . . . H2 H -0.0356 -0.0335 0.1575 0.041 Uiso 1 1 calc R . . C3 C 0.0983(8) 0.0754(6) 0.1288(3) 0.0330(18) Uani 1 1 d . . . C4 C 0.0346(8) -0.0955(7) 0.2544(4) 0.045(2) Uani 1 1 d . . . H4A H 0.0783 -0.1607 0.2493 0.068 Uiso 1 1 calc R . . H4B H -0.061 -0.11 0.2372 0.068 Uiso 1 1 calc R . . H4C H 0.0407 -0.0762 0.2947 0.068 Uiso 1 1 calc R . . C5 C 0.0182(9) 0.0500(7) 0.0700(3) 0.050(2) Uani 1 1 d . . . H5A H 0.0377 0.1111 0.0465 0.075 Uiso 1 1 calc R . . H5B H -0.0791 0.0386 0.0724 0.075 Uiso 1 1 calc R . . H5C H 0.0442 -0.0161 0.0533 0.075 Uiso 1 1 calc R . . C6 C 0.2725(7) 0.0372(6) 0.3079(3) 0.0305(17) Uani 1 1 d . . . C7 C 0.3328(8) -0.0565(6) 0.3149(3) 0.0352(19) Uani 1 1 d . . . H7 H 0.3305 -0.1049 0.283 0.042 Uiso 1 1 calc R . . C8 C 0.3964(8) -0.0819(7) 0.3668(3) 0.040(2) Uani 1 1 d . . . C9 C 0.4034(8) -0.0087(7) 0.4121(3) 0.041(2) Uani 1 1 d . . . H9 H 0.449 -0.0242 0.4478 0.049 Uiso 1 1 calc R . . C10 C 0.3458(8) 0.0870(7) 0.4070(3) 0.038(2) Uani 1 1 d . . . C11 C 0.2843(7) 0.1118(6) 0.3547(3) 0.0311(17) Uani 1 1 d . . . H11 H 0.2499 0.1793 0.3503 0.037 Uiso 1 1 calc R . . C12 C 0.4607(11) -0.1849(8) 0.3732(4) 0.064(3) Uani 1 1 d . . . H12A H 0.5478 -0.1694 0.3983 0.095 Uiso 1 1 calc R . . H12B H 0.4756 -0.2127 0.3362 0.095 Uiso 1 1 calc R . . H12C H 0.4005 -0.2397 0.3893 0.095 Uiso 1 1 calc R . . C13 C 0.3493(10) 0.1656(8) 0.4567(3) 0.059(3) Uani 1 1 d . . . H13A H 0.3898 0.2382 0.4483 0.089 Uiso 1 1 calc R . . H13B H 0.4037 0.1411 0.4898 0.089 Uiso 1 1 calc R . . H13C H 0.2567 0.1688 0.4643 0.089 Uiso 1 1 calc R . . C14 C 0.2560(7) 0.2085(6) 0.0949(3) 0.0296(17) Uani 1 1 d . . . C15 C 0.2753(8) 0.3228(6) 0.0983(3) 0.0362(19) Uani 1 1 d . . . H15 H 0.2458 0.3609 0.1283 0.043 Uiso 1 1 calc R . . C16 C 0.3374(8) 0.3815(7) 0.0583(4) 0.044(2) Uani 1 1 d . . . C17 C 0.3798(9) 0.3265(8) 0.0153(4) 0.051(2) Uani 1 1 d . . . H17 H 0.4199 0.3665 -0.0123 0.062 Uiso 1 1 calc R . . C18 C 0.3655(9) 0.2132(8) 0.0111(3) 0.053(2) Uani 1 1 d . . . C19 C 0.3030(8) 0.1549(7) 0.0514(3) 0.043(2) Uani 1 1 d . . . H19 H 0.2927 0.0775 0.0488 0.051 Uiso 1 1 calc R . . C20 C 0.3545(11) 0.5042(7) 0.0632(4) 0.064(3) Uani 1 1 d . . . H20A H 0.4368 0.5314 0.0897 0.096 Uiso 1 1 calc R . . H20B H 0.2756 0.5285 0.077 0.096 Uiso 1 1 calc R . . H20C H 0.3623 0.5326 0.0261 0.096 Uiso 1 1 calc R . . C21 C 0.4143(12) 0.1514(10) -0.0360(4) 0.084(4) Uani 1 1 d . . . H21A H 0.5122 0.1497 -0.0267 0.125 Uiso 1 1 calc R . . H21B H 0.3955 0.1878 -0.0712 0.125 Uiso 1 1 calc R . . H21C H 0.3668 0.0768 -0.0406 0.125 Uiso 1 1 calc R . . C22 C 0.6501(7) 0.3647(6) 0.2185(3) 0.0289(17) Uani 1 1 d . . . C23 C 0.6308(7) 0.2837(6) 0.1749(3) 0.0297(17) Uani 1 1 d . . . H23 H 0.6301 0.3109 0.1385 0.036 Uiso 1 1 calc R . . C24 C 0.6124(7) 0.1696(6) 0.1750(3) 0.0272(16) Uani 1 1 d . . . C25 C 0.6410(8) 0.4786(6) 0.2002(3) 0.0351(18) Uani 1 1 d . . . H25A H 0.5745 0.5107 0.2194 0.053 Uiso 1 1 calc R . . H25B H 0.6126 0.4764 0.1594 0.053 Uiso 1 1 calc R . . H25C H 0.73 0.5229 0.21 0.053 Uiso 1 1 calc R . . C26 C 0.6306(8) 0.1107(6) 0.1201(3) 0.0370(19) Uani 1 1 d . . . H26A H 0.6897 0.0546 0.1285 0.055 Uiso 1 1 calc R . . H26B H 0.6718 0.1632 0.096 0.055 Uiso 1 1 calc R . . H26C H 0.542 0.0765 0.1005 0.055 Uiso 1 1 calc R . . C27 C 0.7080(7) 0.4354(5) 0.3141(3) 0.0242(15) Uani 1 1 d . . . C28 C 0.8319(7) 0.5024(6) 0.3183(3) 0.0285(17) Uani 1 1 d . . . H28 H 0.8911 0.4912 0.2919 0.034 Uiso 1 1 calc R . . C29 C 0.8704(7) 0.5853(5) 0.3604(3) 0.0259(16) Uani 1 1 d . . . C30 C 0.7810(7) 0.6012(6) 0.3983(3) 0.0315(17) Uani 1 1 d . . . H30 H 0.8055 0.6583 0.4268 0.038 Uiso 1 1 calc R . . C31 C 0.6573(8) 0.5358(6) 0.3952(3) 0.0345(18) Uani 1 1 d . . . C32 C 0.6197(7) 0.4536(6) 0.3521(3) 0.0272(16) Uani 1 1 d . . . H32 H 0.5336 0.4101 0.3487 0.033 Uiso 1 1 calc R . . C33 C 1.0032(7) 0.6592(6) 0.3638(4) 0.040(2) Uani 1 1 d . . . H33A H 0.9991 0.7057 0.3317 0.061 Uiso 1 1 calc R . . H33B H 1.0771 0.6151 0.363 0.061 Uiso 1 1 calc R . . H33C H 1.0195 0.7049 0.399 0.061 Uiso 1 1 calc R . . C34 C 0.5609(9) 0.5538(7) 0.4362(3) 0.046(2) Uani 1 1 d . . . H34A H 0.6051 0.6093 0.4655 0.068 Uiso 1 1 calc R . . H34B H 0.536 0.4854 0.4536 0.068 Uiso 1 1 calc R . . H34C H 0.4791 0.5782 0.4162 0.068 Uiso 1 1 calc R . . C35 C 0.5525(7) -0.0020(6) 0.2116(3) 0.0273(16) Uani 1 1 d . . . C36 C 0.6359(7) -0.0666(6) 0.2421(3) 0.0312(17) Uani 1 1 d . . . H36 H 0.715 -0.0329 0.2661 0.037 Uiso 1 1 calc R . . C37 C 0.6065(7) -0.1794(6) 0.2383(3) 0.0327(18) Uani 1 1 d . . . C38 C 0.4894(7) -0.2268(6) 0.2025(3) 0.0316(18) Uani 1 1 d . . . H38 H 0.4677 -0.3039 0.1989 0.038 Uiso 1 1 calc R . . C39 C 0.4046(7) -0.1628(6) 0.1722(3) 0.0291(17) Uani 1 1 d . . . C40 C 0.4341(7) -0.0517(6) 0.1771(3) 0.0296(17) Uani 1 1 d . . . H40 H 0.3743 -0.0081 0.1571 0.036 Uiso 1 1 calc R . . C41 C 0.6972(8) -0.2483(6) 0.2720(4) 0.042(2) Uani 1 1 d . . . H41A H 0.7555 -0.2783 0.2477 0.064 Uiso 1 1 calc R . . H41B H 0.6416 -0.308 0.2868 0.064 Uiso 1 1 calc R . . H41C H 0.7536 -0.2035 0.3033 0.064 Uiso 1 1 calc R . . C42 C 0.2758(8) -0.2148(6) 0.1336(3) 0.042(2) Uani 1 1 d . . . H42A H 0.205 -0.1674 0.134 0.063 Uiso 1 1 calc R . . H42B H 0.2444 -0.2859 0.1469 0.063 Uiso 1 1 calc R . . H42C H 0.2954 -0.2243 0.0951 0.063 Uiso 1 1 calc R . . C43 C 1.1621(7) 0.4556(6) 0.2667(3) 0.0311(17) Uani 1 1 d . . . C44 C 1.1940(7) 0.4392(6) 0.3243(3) 0.0335(18) Uani 1 1 d . . . H44 H 1.279 0.4772 0.3416 0.04 Uiso 1 1 calc R . . C45 C 1.1234(7) 0.3766(6) 0.3613(3) 0.0316(17) Uani 1 1 d . . . C46 C 1.2596(8) 0.5427(7) 0.2451(4) 0.042(2) Uani 1 1 d . . . H46A H 1.2669 0.5234 0.2059 0.063 Uiso 1 1 calc R . . H46B H 1.3493 0.5478 0.2682 0.063 Uiso 1 1 calc R . . H46C H 1.2256 0.6131 0.2475 0.063 Uiso 1 1 calc R . . C47 C 1.1702(9) 0.4076(7) 0.4238(4) 0.050(2) Uani 1 1 d . . . H47A H 1.1167 0.462 0.4364 0.074 Uiso 1 1 calc R . . H47B H 1.2664 0.438 0.4298 0.074 Uiso 1 1 calc R . . H47C H 1.1577 0.3426 0.4454 0.074 Uiso 1 1 calc R . . C48 C 0.9550(7) 0.2407(6) 0.3850(3) 0.0291(17) Uani 1 1 d . . . C49 C 0.9516(8) 0.1272(6) 0.3860(3) 0.0360(19) Uani 1 1 d . . . H49 H 0.9981 0.0904 0.3611 0.043 Uiso 1 1 calc R . . C50 C 0.8822(8) 0.0690(6) 0.4224(3) 0.0364(19) Uani 1 1 d . . . C51 C 0.8121(8) 0.1226(7) 0.4585(3) 0.042(2) Uani 1 1 d . . . H51 H 0.765 0.0822 0.4841 0.05 Uiso 1 1 calc R . . C52 C 0.8103(8) 0.2353(7) 0.4575(3) 0.0361(19) Uani 1 1 d . . . C53 C 0.8815(7) 0.2934(6) 0.4196(3) 0.0336(18) Uani 1 1 d . . . H53 H 0.8793 0.3696 0.4177 0.04 Uiso 1 1 calc R . . C54 C 0.8849(11) -0.0531(7) 0.4242(4) 0.061(3) Uani 1 1 d . . . H54A H 0.9547 -0.0742 0.4031 0.091 Uiso 1 1 calc R . . H54B H 0.7961 -0.0918 0.4074 0.091 Uiso 1 1 calc R . . H54C H 0.9055 -0.0722 0.4635 0.091 Uiso 1 1 calc R . . C55 C 0.7280(9) 0.2923(8) 0.4936(4) 0.056(3) Uani 1 1 d . . . H55A H 0.7172 0.2512 0.5271 0.085 Uiso 1 1 calc R . . H55B H 0.6385 0.2971 0.4721 0.085 Uiso 1 1 calc R . . H55C H 0.7746 0.3658 0.5053 0.085 Uiso 1 1 calc R . . C56 C 1.0100(7) 0.4415(7) 0.1803(3) 0.0338(19) Uani 1 1 d . . . C57 C 0.9817(7) 0.5471(6) 0.1753(3) 0.0346(18) Uani 1 1 d . . . H57 H 1.0023 0.5966 0.2075 0.042 Uiso 1 1 calc R . . C58 C 0.9232(8) 0.5834(7) 0.1238(4) 0.039(2) Uani 1 1 d . . . C59 C 0.8976(8) 0.5102(8) 0.0767(4) 0.050(2) Uani 1 1 d . . . H59 H 0.8614 0.5342 0.0413 0.059 Uiso 1 1 calc R . . C60 C 0.9232(9) 0.4047(7) 0.0803(4) 0.044(2) Uani 1 1 d . . . C61 C 0.9783(8) 0.3688(7) 0.1321(3) 0.040(2) Uani 1 1 d . . . H61 H 0.9944 0.2952 0.1348 0.049 Uiso 1 1 calc R . . C62 C 0.8887(10) 0.6989(7) 0.1197(4) 0.057(2) Uani 1 1 d . . . H62A H 0.8824 0.7188 0.0804 0.086 Uiso 1 1 calc R . . H62B H 0.9599 0.7492 0.1432 0.086 Uiso 1 1 calc R . . H62C H 0.8017 0.7031 0.1328 0.086 Uiso 1 1 calc R . . C63 C 0.8957(12) 0.3254(8) 0.0278(4) 0.073(3) Uani 1 1 d . . . H63A H 0.8254 0.2656 0.0328 0.11 Uiso 1 1 calc R . . H63B H 0.9792 0.296 0.0227 0.11 Uiso 1 1 calc R . . H63C H 0.8648 0.3641 -0.0054 0.11 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl1 0.02473(16) 0.03041(17) 0.02932(17) -0.00278(12) 0.00150(11) 0.00053(12) Tl2 0.02847(17) 0.02764(17) 0.02850(17) 0.00000(12) 0.00075(12) -0.00124(12) Tl3 0.02462(16) 0.02888(18) 0.0412(2) -0.00166(13) 0.00337(13) -0.00085(12) N1 0.028(3) 0.031(3) 0.023(3) -0.004(3) 0.002(3) -0.003(3) N2 0.036(4) 0.027(4) 0.027(3) -0.001(3) 0.000(3) 0.006(3) N3 0.018(3) 0.031(4) 0.033(4) -0.006(3) 0.001(3) 0.001(3) N4 0.031(3) 0.020(3) 0.029(3) -0.002(3) 0.001(3) 0.005(3) N5 0.019(3) 0.039(4) 0.040(4) -0.003(3) 0.006(3) 0.004(3) N6 0.028(3) 0.028(4) 0.035(4) 0.004(3) 0.002(3) -0.001(3) C1 0.030(4) 0.030(4) 0.033(4) 0.001(3) 0.006(3) 0.008(3) C2 0.031(4) 0.026(4) 0.039(5) -0.005(3) -0.004(3) -0.003(3) C3 0.040(5) 0.027(4) 0.031(4) -0.005(3) -0.001(3) 0.014(4) C4 0.044(5) 0.041(5) 0.049(5) -0.002(4) 0.014(4) -0.012(4) C5 0.058(6) 0.047(5) 0.035(5) -0.002(4) -0.014(4) -0.004(4) C6 0.027(4) 0.040(5) 0.025(4) 0.002(3) 0.009(3) 0.002(3) C7 0.048(5) 0.034(5) 0.026(4) 0.000(3) 0.012(4) 0.008(4) C8 0.051(5) 0.051(5) 0.028(5) 0.013(4) 0.018(4) 0.023(4) C9 0.039(5) 0.056(6) 0.031(5) 0.015(4) 0.001(4) 0.018(4) C10 0.029(4) 0.063(6) 0.022(4) -0.007(4) 0.008(3) 0.001(4) C11 0.027(4) 0.033(4) 0.032(4) -0.001(3) 0.004(3) 0.001(3) C12 0.090(8) 0.076(7) 0.035(5) 0.012(5) 0.015(5) 0.042(6) C13 0.082(8) 0.067(7) 0.029(5) -0.001(4) -0.001(5) 0.017(6) C14 0.029(4) 0.036(5) 0.024(4) 0.001(3) 0.003(3) 0.005(3) C15 0.041(5) 0.038(5) 0.025(4) -0.002(3) -0.005(3) 0.003(4) C16 0.043(5) 0.046(5) 0.040(5) 0.008(4) 0.006(4) -0.006(4) C17 0.059(6) 0.055(6) 0.041(5) 0.008(4) 0.014(4) 0.003(5) C18 0.056(6) 0.075(7) 0.031(5) 0.003(5) 0.014(4) 0.016(5) C19 0.051(5) 0.040(5) 0.038(5) -0.004(4) 0.005(4) 0.014(4) C20 0.082(8) 0.054(6) 0.046(6) 0.015(5) -0.001(5) -0.024(5) C21 0.111(10) 0.104(10) 0.049(7) -0.007(6) 0.038(6) 0.037(8) C22 0.019(4) 0.026(4) 0.040(5) 0.000(3) 0.003(3) -0.001(3) C23 0.033(4) 0.025(4) 0.033(4) 0.002(3) 0.006(3) 0.010(3) C24 0.023(4) 0.024(4) 0.033(4) -0.005(3) -0.001(3) 0.003(3) C25 0.036(4) 0.035(5) 0.032(4) -0.001(3) -0.002(3) 0.006(4) C26 0.043(5) 0.040(5) 0.029(4) -0.007(4) 0.009(4) 0.005(4) C27 0.024(4) 0.023(4) 0.023(4) -0.003(3) -0.002(3) 0.000(3) C28 0.037(4) 0.024(4) 0.027(4) 0.005(3) 0.005(3) 0.013(3) C29 0.021(4) 0.019(4) 0.034(4) 0.003(3) -0.006(3) 0.001(3) C30 0.032(4) 0.029(4) 0.030(4) -0.004(3) -0.004(3) 0.004(3) C31 0.040(5) 0.030(4) 0.033(5) -0.005(3) 0.005(3) 0.009(4) C32 0.020(4) 0.032(4) 0.028(4) 0.000(3) -0.001(3) 0.002(3) C33 0.030(4) 0.033(5) 0.052(5) -0.003(4) -0.006(4) -0.003(4) C34 0.050(5) 0.046(5) 0.042(5) -0.004(4) 0.014(4) 0.005(4) C35 0.028(4) 0.024(4) 0.030(4) -0.004(3) 0.007(3) 0.002(3) C36 0.021(4) 0.028(4) 0.043(5) -0.005(3) 0.003(3) -0.001(3) C37 0.031(4) 0.030(4) 0.036(5) -0.002(3) 0.006(3) 0.000(3) C38 0.035(4) 0.017(4) 0.044(5) -0.004(3) 0.013(4) 0.001(3) C39 0.031(4) 0.029(4) 0.026(4) -0.007(3) 0.008(3) -0.001(3) C40 0.029(4) 0.027(4) 0.033(4) -0.001(3) 0.007(3) 0.006(3) C41 0.043(5) 0.021(4) 0.061(6) -0.006(4) 0.005(4) 0.005(4) C42 0.042(5) 0.027(4) 0.049(5) -0.012(4) -0.006(4) -0.005(4) C43 0.018(4) 0.032(4) 0.045(5) 0.002(4) 0.007(3) 0.007(3) C44 0.021(4) 0.031(4) 0.047(5) 0.003(4) 0.002(3) 0.002(3) C45 0.024(4) 0.028(4) 0.042(5) 0.002(3) -0.002(3) 0.008(3) C46 0.031(4) 0.042(5) 0.052(5) 0.001(4) 0.009(4) -0.003(4) C47 0.044(5) 0.044(5) 0.053(6) 0.004(4) -0.006(4) -0.010(4) C48 0.026(4) 0.026(4) 0.034(4) 0.001(3) 0.002(3) 0.001(3) C49 0.035(5) 0.027(4) 0.044(5) 0.002(4) 0.002(4) 0.002(3) C50 0.040(5) 0.032(5) 0.034(5) 0.005(4) 0.001(4) -0.001(4) C51 0.040(5) 0.050(6) 0.034(5) 0.021(4) 0.003(4) -0.006(4) C52 0.034(4) 0.047(5) 0.027(4) 0.004(4) -0.003(3) 0.007(4) C53 0.025(4) 0.036(5) 0.037(5) -0.001(4) -0.003(3) 0.001(3) C54 0.078(7) 0.039(5) 0.060(6) 0.015(5) 0.006(5) -0.009(5) C55 0.050(6) 0.070(7) 0.050(6) 0.006(5) 0.014(5) 0.003(5) C56 0.015(4) 0.047(5) 0.038(5) -0.007(4) 0.006(3) -0.001(3) C57 0.025(4) 0.030(4) 0.049(5) 0.004(4) 0.008(4) 0.002(3) C58 0.026(4) 0.037(5) 0.051(5) 0.007(4) -0.004(4) 0.001(4) C59 0.039(5) 0.064(7) 0.039(5) -0.004(5) -0.007(4) 0.001(4) C60 0.044(5) 0.042(5) 0.044(5) 0.004(4) 0.010(4) 0.001(4) C61 0.030(4) 0.044(5) 0.045(5) -0.003(4) 0.008(4) -0.006(4) C62 0.061(6) 0.044(6) 0.065(6) 0.007(5) -0.002(5) 0.015(5) C63 0.108(9) 0.057(7) 0.047(6) -0.014(5) -0.008(6) 0.009(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N2 2.462(6) . ? Tl1 N1 2.472(6) . ? Tl1 Tl2 3.5794(4) . ? Tl2 N4 2.504(6) . ? Tl2 N3 2.520(6) . ? Tl2 Tl3 3.7977(4) . ? Tl3 N5 2.482(6) . ? Tl3 N6 2.515(6) . ? N1 C1 1.318(9) . ? N1 C6 1.416(9) . ? N2 C3 1.329(9) . ? N2 C14 1.412(9) . ? N3 C22 1.349(9) . ? N3 C27 1.423(8) . ? N4 C24 1.331(9) . ? N4 C35 1.429(9) . ? N5 C43 1.327(9) . ? N5 C56 1.407(10) . ? N6 C45 1.315(9) . ? N6 C48 1.418(9) . ? C1 C2 1.411(10) . ? C1 C4 1.534(10) . ? C2 C3 1.401(11) . ? C2 H2 0.95 . ? C3 C5 1.521(10) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C7 1.383(10) . ? C6 C11 1.408(10) . ? C7 C8 1.384(11) . ? C7 H7 0.95 . ? C8 C9 1.378(11) . ? C8 C12 1.507(11) . ? C9 C10 1.388(11) . ? C9 H9 0.95 . ? C10 C11 1.381(11) . ? C10 C13 1.506(11) . ? C11 H11 0.95 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 C19 1.389(10) . ? C14 C15 1.402(10) . ? C15 C16 1.399(11) . ? C15 H15 0.95 . ? C16 C17 1.364(11) . ? C16 C20 1.508(12) . ? C17 C18 1.392(12) . ? C17 H17 0.95 . ? C18 C19 1.405(12) . ? C18 C21 1.516(11) . ? C19 H19 0.95 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C23 1.396(10) . ? C22 C25 1.505(10) . ? C23 C24 1.404(10) . ? C23 H23 0.95 . ? C24 C26 1.530(9) . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C28 1.394(9) . ? C27 C32 1.395(9) . ? C28 C29 1.389(9) . ? C28 H28 0.95 . ? C29 C30 1.395(10) . ? C29 C33 1.509(9) . ? C30 C31 1.386(10) . ? C30 H30 0.95 . ? C31 C32 1.399(9) . ? C31 C34 1.509(10) . ? C32 H32 0.95 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 C36 1.385(10) . ? C35 C40 1.402(10) . ? C36 C37 1.390(10) . ? C36 H36 0.95 . ? C37 C38 1.400(10) . ? C37 C41 1.501(11) . ? C38 C39 1.386(10) . ? C38 H38 0.95 . ? C39 C40 1.369(10) . ? C39 C42 1.531(10) . ? C40 H40 0.95 . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 C44 1.403(11) . ? C43 C46 1.522(10) . ? C44 C45 1.413(10) . ? C44 H44 0.95 . ? C45 C47 1.526(11) . ? C46 H46A 0.98 . ? C46 H46B 0.98 . ? C46 H46C 0.98 . ? C47 H47A 0.98 . ? C47 H47B 0.98 . ? C47 H47C 0.98 . ? C48 C53 1.388(10) . ? C48 C49 1.404(10) . ? C49 C50 1.368(10) . ? C49 H49 0.95 . ? C50 C51 1.395(11) . ? C50 C54 1.520(11) . ? C51 C52 1.401(11) . ? C51 H51 0.95 . ? C52 C53 1.402(10) . ? C52 C55 1.499(11) . ? C53 H53 0.95 . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? C55 H55A 0.98 . ? C55 H55B 0.98 . ? C55 H55C 0.98 . ? C56 C57 1.382(11) . ? C56 C61 1.411(10) . ? C57 C58 1.407(11) . ? C57 H57 0.95 . ? C58 C59 1.394(11) . ? C58 C62 1.518(11) . ? C59 C60 1.369(12) . ? C59 H59 0.95 . ? C60 C61 1.401(12) . ? C60 C63 1.537(11) . ? C61 H61 0.95 . ? C62 H62A 0.98 . ? C62 H62B 0.98 . ? C62 H62C 0.98 . ? C63 H63A 0.98 . ? C63 H63B 0.98 . ? C63 H63C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Tl1 N1 75.94(19) . . ? N2 Tl1 Tl2 133.51(14) . . ? N1 Tl1 Tl2 86.13(14) . . ? N4 Tl2 N3 75.77(18) . . ? N4 Tl2 Tl1 59.77(13) . . ? N3 Tl2 Tl1 68.80(13) . . ? N4 Tl2 Tl3 63.57(13) . . ? N3 Tl2 Tl3 56.99(12) . . ? Tl1 Tl2 Tl3 107.908(10) . . ? N5 Tl3 N6 76.81(19) . . ? N5 Tl3 Tl2 128.78(13) . . ? N6 Tl3 Tl2 79.23(13) . . ? C1 N1 C6 120.8(6) . . ? C1 N1 Tl1 129.9(5) . . ? C6 N1 Tl1 109.2(4) . . ? C3 N2 C14 121.4(6) . . ? C3 N2 Tl1 130.3(5) . . ? C14 N2 Tl1 108.3(4) . . ? C22 N3 C27 119.1(6) . . ? C22 N3 Tl2 128.8(4) . . ? C27 N3 Tl2 110.2(4) . . ? C24 N4 C35 118.7(6) . . ? C24 N4 Tl2 130.0(4) . . ? C35 N4 Tl2 109.9(4) . . ? C43 N5 C56 120.9(6) . . ? C43 N5 Tl3 127.8(5) . . ? C56 N5 Tl3 111.3(4) . . ? C45 N6 C48 121.0(6) . . ? C45 N6 Tl3 128.4(5) . . ? C48 N6 Tl3 110.5(4) . . ? N1 C1 C2 125.5(7) . . ? N1 C1 C4 120.1(7) . . ? C2 C1 C4 114.3(6) . . ? C3 C2 C1 129.9(7) . . ? C3 C2 H2 115 . . ? C1 C2 H2 115 . . ? N2 C3 C2 124.8(7) . . ? N2 C3 C5 121.5(7) . . ? C2 C3 C5 113.7(7) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 118.4(7) . . ? C7 C6 N1 122.8(6) . . ? C11 C6 N1 118.6(7) . . ? C6 C7 C8 122.0(7) . . ? C6 C7 H7 119 . . ? C8 C7 H7 119 . . ? C9 C8 C7 118.2(7) . . ? C9 C8 C12 120.9(7) . . ? C7 C8 C12 120.9(7) . . ? C8 C9 C10 121.7(7) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C11 C10 C9 119.3(7) . . ? C11 C10 C13 118.7(8) . . ? C9 C10 C13 121.9(8) . . ? C10 C11 C6 120.2(7) . . ? C10 C11 H11 119.9 . . ? C6 C11 H11 119.9 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 118.2(7) . . ? C19 C14 N2 123.7(7) . . ? C15 C14 N2 117.8(6) . . ? C16 C15 C14 121.1(7) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C17 C16 C15 119.4(8) . . ? C17 C16 C20 121.4(8) . . ? C15 C16 C20 119.3(8) . . ? C16 C17 C18 121.5(8) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C19 118.8(8) . . ? C17 C18 C21 121.9(9) . . ? C19 C18 C21 119.4(9) . . ? C14 C19 C18 121.1(8) . . ? C14 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 C23 123.9(7) . . ? N3 C22 C25 120.5(6) . . ? C23 C22 C25 115.5(7) . . ? C22 C23 C24 132.0(7) . . ? C22 C23 H23 114 . . ? C24 C23 H23 114 . . ? N4 C24 C23 124.2(6) . . ? N4 C24 C26 120.8(6) . . ? C23 C24 C26 114.9(6) . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 119.3(6) . . ? C28 C27 N3 120.3(6) . . ? C32 C27 N3 120.3(6) . . ? C29 C28 C27 121.3(6) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C29 C30 118.3(6) . . ? C28 C29 C33 121.0(6) . . ? C30 C29 C33 120.6(6) . . ? C31 C30 C29 121.7(6) . . ? C31 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C30 C31 C32 119.1(6) . . ? C30 C31 C34 121.4(6) . . ? C32 C31 C34 119.5(7) . . ? C27 C32 C31 120.3(6) . . ? C27 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C29 C33 H33A 109.5 . . ? C29 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C29 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 119.2(7) . . ? C36 C35 N4 119.8(6) . . ? C40 C35 N4 120.8(7) . . ? C35 C36 C37 121.5(7) . . ? C35 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C36 C37 C38 118.0(7) . . ? C36 C37 C41 120.9(7) . . ? C38 C37 C41 121.1(7) . . ? C39 C38 C37 120.9(7) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C40 C39 C38 120.3(7) . . ? C40 C39 C42 118.9(7) . . ? C38 C39 C42 120.8(7) . . ? C39 C40 C35 120.0(7) . . ? C39 C40 H40 120 . . ? C35 C40 H40 120 . . ? C37 C41 H41A 109.5 . . ? C37 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C37 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N5 C43 C44 124.9(7) . . ? N5 C43 C46 120.8(7) . . ? C44 C43 C46 114.3(7) . . ? C43 C44 C45 132.0(7) . . ? C43 C44 H44 114 . . ? C45 C44 H44 114 . . ? N6 C45 C44 124.6(7) . . ? N6 C45 C47 120.3(7) . . ? C44 C45 C47 115.1(7) . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C53 C48 C49 119.3(7) . . ? C53 C48 N6 122.6(7) . . ? C49 C48 N6 117.9(6) . . ? C50 C49 C48 120.9(7) . . ? C50 C49 H49 119.5 . . ? C48 C49 H49 119.5 . . ? C49 C50 C51 119.6(7) . . ? C49 C50 C54 119.9(8) . . ? C51 C50 C54 120.5(7) . . ? C50 C51 C52 120.8(7) . . ? C50 C51 H51 119.6 . . ? C52 C51 H51 119.6 . . ? C51 C52 C53 118.6(7) . . ? C51 C52 C55 121.0(7) . . ? C53 C52 C55 120.3(8) . . ? C48 C53 C52 120.6(7) . . ? C48 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C50 C54 H54A 109.5 . . ? C50 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C50 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 N5 123.1(7) . . ? C57 C56 C61 118.4(8) . . ? N5 C56 C61 118.3(7) . . ? C56 C57 C58 121.9(7) . . ? C56 C57 H57 119.1 . . ? C58 C57 H57 119.1 . . ? C59 C58 C57 118.0(8) . . ? C59 C58 C62 121.1(8) . . ? C57 C58 C62 120.9(7) . . ? C60 C59 C58 121.7(8) . . ? C60 C59 H59 119.2 . . ? C58 C59 H59 119.2 . . ? C59 C60 C61 119.7(8) . . ? C59 C60 C63 121.0(8) . . ? C61 C60 C63 119.3(8) . . ? C60 C61 C56 120.3(8) . . ? C60 C61 H61 119.9 . . ? C56 C61 H61 119.9 . . ? C58 C62 H62A 109.5 . . ? C58 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C58 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? #===END