#\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2014-02-11 at 21:23:28 # Using CIFtbx version 3.0.4 1 Sep 2006 # Dictionary name : cif_core.dic # Dictionary vers : 2.4.3 # Request file : c:\wingx\files\acta.reqdat # CIF files read : 1132 psiabs stdanal struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_global #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2014-02-11 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? # PROCESSING SUMMARY (IUCr Office Use Only) _journal_data_validation_number ? _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # # SUBMISSION DETAILS # Name and address of author for correspondence _publ_contact_author_name 'Bényei, Attila Csaba' _publ_contact_author_address ; University of Debrecen 1 Egyetem tér Debrecen Hungary H-4032 ; _publ_contact_author_email 'benyei.attila@science.unideb.hu' _publ_contact_author_fax ' ' _publ_contact_author_phone '+3652512900 ext 22486' _publ_contact_letter ; Submission dated :2014-02-11 Please consider this CIF as a supplement to our paper. I certify that all authors have seen and approved of this submission, that all have made significant scientific contributions to the work reported, and that all share responsibility and accountability for the results. The CIF has passed the Chester CHECKCIF routines and all possible Alerts have been responded to. The CIF also gives a satisfactory PRINTCIF file. Attila Benyei ; _publ_requested_journal 'Acta Cryst C' _publ_requested_category ? # one of FI/FM/FO #============================================================================== # # TITLE AND AUTHOR LIST _publ_section_title ; An extraordinary robust macrocyclic complex, the Tl(III)DOTA-: chemical characterization of equilibrium, kinetics and structure ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Tam\'as Fodor' ? ; University of Debrecen, Department of Inorganic and Analytical Chemistry, H-4032 Debrecen, Egyetem t\'er 1, Hungary ; 'Istv\'an B\'anyai' ? ; University of Debrecen, Department of Colloid and Environmental Chemistry, H-4032 Debrecen, Egyetem t\'er 1, Hungary ; 'Attila B\'enyei' ? ; University of Debrecen, Department of Physical Chemistry, H-4032 Debrecen, Egyetem t\'er 1, Hungary ; 'Carlos Platas-Iglesias' ? ; Departamento de Qu\'imica Fundamental, Facultade de Ciencias, Universidade da Coru\~na, Campus da Zapateira-R\'ua da Fraga 10, 15008 A Coru\~na, Spain ; 'Mih\'aly Purgel' ? ; MTA-DE Homogeneous Catalysis and Reaction Mechanisms Research Group, H-4032 Debrecen, Egyetem t\'er 1, Hungary ; 'G\'abor Horv\'ath' ? ; University of Debrecen, Department of Inorganic and Analytical Chemistry, H-4032 Debrecen, Egyetem t\'er 1, Hungary Institute of Innate Immunity Biomedical Center, University Hospitals, University of Bonn, Germany ; 'L\'aszl\'o Z\'ek\'any' ? ; University of Debrecen, Department of Inorganic and Analytical Chemistry, H-4032 Debrecen, Egyetem t\'er 1, Hungary ; 'Gyula Tircs\'o' ? ; University of Debrecen, Department of Inorganic and Analytical Chemistry, H-4032 Debrecen, Egyetem t\'er 1, Hungary ; 'Imre T\'oth' ? ; University of Debrecen, Department of Inorganic and Analytical Chemistry, H-4032 Debrecen, Egyetem t\'er 1, Hungary ; #============================================================================== # # TEXT _publ_section_synopsis ; ? ; # A synopsis (< 40 words) in place of the ? character is REQUIRED for # inorganic structure papers in Acta Cryst C. # _publ_section_abstract ; ? ; # Replace the ? character with a concise structurally-informative abstract # The abstract should state the formula and systematic compound name if not # already in the title. It should also report any crystallographic symmetry # (not 1) required of the structure by the space group. Do not give crystal # data here. # ----------------------------------------------------------------------------- _publ_section_comment ; ? ; # For Acta C submissions, replace the ? character with an informative Comment # section which provides significant added value to the numerical data freely # available in the CIF. # _publ_section_acknowledgements ; ? ; # Replace the ? character with any acknowledgements. # _publ_section_related_literature ; ? ; _publ_section_references ; # # Put here all your general crystallographic references # Unecessary ones can be deleted from the document CIF # MACH3/PC Software: Enraf-Nonius (1992). CAD-4 Software (or CAD-4 EXPRESS). Enraf-Nonius, Delft, The Netherlands. Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388. CAMERON: Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON. Chemical Crystallography Laboratory, Oxford, England. enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338. MERCURY: Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470. MOGUL: Bruno, I. J., Cole, J. C., Kessler, M., Luo, J., Motherwell, W. D. S., Purkis, L. H., Smith, B. R., Taylor, R., Cooper, R. I., Harris, S. E. & Orpen, A. G. (2004). J. Chem. Inf. Comput. Sci. 44, 2133-2144. ORTEPII: Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. ORTEPIII: Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. ORTEP-3: Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854. PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659. PLATON: Spek, A. L. (2009). Acta. Cryst. D65, 148-155. PublCIF: Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925. SHELX: Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SIR92: Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. WinGX: Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854. XCAD4: Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany. ; # List of references should be in alphabetical sequence with one blank # line between each reference. See Notes for Authors for full # specifications as to how references should be presented. # Scattering-factor references are not needed here # ----------------------------------------------------------------------------- _publ_section_figure_captions ; ? ; # Replace the '?" character with e.g. # "Fig. 1. A view of (1). Displacement ellipsoids are drawn at the 30% # probability level." # ----------------------------------------------------------------------------- _publ_section_table_legends ; ? ; # Replace the '?" character with e.g. # "Table 1. Selected geometric parameters (\%A, \%) for compound (1)." # # "Table 2. Hydrogen-bond parameters (\%A, \%) for compound (1)." # # ----------------------------------------------------------------------------- _publ_section_exptl_prep ; ? ; # Replace the ? character with concise details including reagent quantities # and reaction conditions of compound preparation. A reference may suffice, # but do give sufficient brief details if the method is unpublished or # deviates from a published method. Also give the crystallisation procedure # and solvent(s). This is a good place to give any physical details such as # analytical and supportive spectroscopic data, and melting point if known. # Long lists of spectroscopic data should not be given here but should be # placed in the _exptl_special_details section of the CIF. # ----------------------------------------------------------------------------- _publ_section_exptl_refinement ; ? ; # Replace the ? character with concise details of any UNUSUAL aspects of the # data collection and structure analysis. # If H atoms were not treated as "constrained", details of how they were # allowed for and range of refined X-H distances MUST be given here. For # constrained X-H distances, report the ranges of the various X-H dimensions # and treatment of U(H). # Routine statements about data collection and processing, structure # solution methods or anisotropic refinement should NOT be given here # (this information is generated automatically from other details in the # CIF). # Note that if RESTRAINTS are used in the refinement, concise details # of what these were should either be given here or in the # _refinement_special # #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_TlDOTA _audit_creation_date 2014-02-11T21:23:28-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H24 N4 O8 Tl1, C H6 N3, H2 O' _chemical_formula_sum 'C17 H32 N7 O9 Tl' _chemical_formula_weight 682.86 #============================================================================== # CRYSTAL DATA _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.498(10) _cell_length_b 12.406(5) _cell_length_c 12.800(4) _cell_angle_alpha 91.010(10) _cell_angle_beta 90.86(4) _cell_angle_gamma 107.31(6) _cell_volume 1136.3(17) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.4 _cell_measurement_theta_max 15.3 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.996 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 7.172 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 3 Theta correction was applied. Averaged transmission function was used. Fourier smoothing - Window value 5 ; _exptl_absorpt_correction_T_min 0.5562 _exptl_absorpt_correction_T_max 0.9874 #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device 'Enraf-Nonius MACH3' _diffrn_measurement_method omega-theta-scans _diffrn_reflns_number 4909 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_theta_min 2.846 _diffrn_reflns_theta_max 26.011 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 3 _diffrn_standards_interval_count 182 _diffrn_standards_interval_time 109 _diffrn_standards_decay_% 10 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -3 -1 -2 -1 -3 -3 5 -3 #============================================================================== # STRUCTURE SOLUTION _atom_sites_solution_hydrogens mixed #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 4464 _reflns_number_gt 4117 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1557 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.087 _refine_ls_number_reflns 4464 _refine_ls_number_parameters 331 _refine_ls_number_restraints 19 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0992P)^2^+10.8511P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.575 _refine_diff_density_min -4.053 _refine_diff_density_rms 0.303 _refine_ls_extinction_method none 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' O O 0.0106 0.006 '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' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol C1 0.9354(16) 0.8563(8) 0.7617(8) 0.035(2) Uani d 1 . . C C2 0.7485(18) 0.3391(10) 0.9621(8) 0.041(3) Uani d 1 . . C H2A 0.8435 0.3395 1.0145 0.049 Uiso calc 1 . . H H2B 0.6372 0.3421 0.9981 0.049 Uiso calc 1 . . H C3 0.8178(17) 0.4441(10) 0.8952(8) 0.038(2) Uani d 1 . . C H3A 0.841 0.5113 0.9395 0.046 Uiso calc 1 . . H H3B 0.9349 0.4445 0.8636 0.046 Uiso calc 1 . . H C5 0.7666(18) 0.5221(9) 0.7293(9) 0.038(3) Uani d 1 . . C H5A 0.8606 0.5868 0.7601 0.046 Uiso calc 1 . . H H5B 0.6731 0.5494 0.6946 0.046 Uiso calc 1 . . H C6 0.8572(17) 0.4651(9) 0.6489(8) 0.039(3) Uani d 1 . . C H6A 0.9044 0.5175 0.5933 0.046 Uiso calc 1 . . H H6B 0.9633 0.4486 0.6817 0.046 Uiso calc 1 . . H C8 0.8381(17) 0.2923(9) 0.5533(8) 0.037(2) Uani d 1 . . C H8A 0.9419 0.3416 0.5164 0.044 Uiso calc 1 . . H H8B 0.7575 0.2414 0.5021 0.044 Uiso calc 1 . . H C9 0.9134(15) 0.2235(9) 0.6299(9) 0.035(2) Uani d 1 . . C H9A 0.9757 0.1774 0.5917 0.042 Uiso calc 1 . . H H9B 1.0049 0.2742 0.6766 0.042 Uiso calc 1 . . H C10 0.6569(17) 0.0509(9) 0.6278(9) 0.039(2) Uani d 1 . . C H10C 0.7281 -0.0027 0.6236 0.046 Uiso calc 1 . . H H10D 0.6397 0.0743 0.5574 0.046 Uiso calc 1 . . H C11 0.8439(18) 0.1164(10) 0.7852(10) 0.042(3) Uani d 1 . . C H11A 0.9618 0.1037 0.7681 0.051 Uiso calc 1 . . H H11B 0.7603 0.0455 0.8084 0.051 Uiso calc 1 . . H C12 0.8768(16) 0.2039(10) 0.8739(9) 0.039(3) Uani d 1 . . C H12A 0.9217 0.1744 0.9353 0.046 Uiso calc 1 . . H H12B 0.9733 0.2714 0.8541 0.046 Uiso calc 1 . . H C41 0.5218(17) 0.4778(10) 0.8551(10) 0.039(3) Uani d 1 . . C H41A 0.559 0.5588 0.8682 0.047 Uiso calc 1 . . H H41B 0.4901 0.4412 0.9215 0.047 Uiso calc 1 . . H C42 0.3474(17) 0.4443(10) 0.7821(11) 0.043(3) Uani d 1 . . C C71 0.593(2) 0.3835(11) 0.5302(9) 0.044(3) Uani d 1 . . C H71A 0.6512 0.4046 0.4633 0.053 Uiso calc 1 . . H H71B 0.5575 0.4473 0.5574 0.053 Uiso calc 1 . . H C72 0.4219(19) 0.2862(11) 0.5131(9) 0.044(3) Uani d 1 . . C C100 0.4686(16) -0.0062(10) 0.6728(9) 0.036(2) Uani d 1 . . C C111 0.5725(18) 0.1443(11) 0.9568(9) 0.044(3) Uani d 1 . . C H11C 0.6099 0.1493 1.0301 0.052 Uiso calc 1 . . H H11D 0.5768 0.0718 0.9292 0.052 Uiso calc 1 . . H C112 0.3713(15) 0.1499(9) 0.9478(8) 0.034(2) Uani d 1 . . C N1 0.7059(12) 0.2347(8) 0.9006(6) 0.0305(19) Uani d 1 . . N N4 0.6791(12) 0.4467(7) 0.8115(7) 0.0305(18) Uani d 1 . . N N7 0.7332(12) 0.3608(7) 0.6029(7) 0.0308(18) Uani d 1 . . N N10 0.7639(12) 0.1507(7) 0.6913(6) 0.0275(17) Uani d 1 . . N N11 0.7586(16) 0.8112(9) 0.7831(8) 0.048(3) Uani d 1 . . N N12 1.0543(15) 0.9125(8) 0.8368(7) 0.041(2) Uani d 1 . . N N13 0.9945(16) 0.8446(11) 0.6683(9) 0.055(3) Uani d 1 . . N O1 0.3317(12) 0.2100(7) 0.8757(6) 0.0424(19) Uani d 1 . . O O2 0.2598(13) 0.0954(8) 1.0105(7) 0.052(2) Uani d 1 . . O O1W 1.348(3) 0.7297(11) 0.7958(12) 0.100(5) Uani d 1 . . O O11 0.4059(11) 0.0465(7) 0.7413(6) 0.0413(19) Uani d 1 . . O O12 0.3860(12) -0.1033(7) 0.6392(7) 0.045(2) Uani d 1 . . O O41 0.3353(13) 0.3653(8) 0.7172(7) 0.050(2) Uani d 1 . . O O42 0.2310(13) 0.4933(9) 0.7988(10) 0.066(3) Uani d 1 . . O O71 0.3892(12) 0.2021(7) 0.5772(6) 0.0420(19) Uani d 1 . . O O72 0.3207(15) 0.2910(9) 0.4378(8) 0.065(3) Uani d 1 . . O Tl1 0.53838(4) 0.25126(3) 0.73845(2) 0.02369(16) Uani d 1 . . Tl H1A 1.375(16) 0.768(9) 0.741(5) 0.028 Uiso d 1 . . H H1B 1.287(14) 0.659(3) 0.789(9) 0.028 Uiso d 1 . . H H10A 0.732(14) 0.824(6) 0.851(3) 0.028 Uiso d 1 . . H H10B 0.710(4) 0.777(4) 0.721(3) 0.028 Uiso d 1 . . H H20A 1.173(7) 0.941(6) 0.816(7) 0.028 Uiso d 1 . . H H20B 0.978(11) 0.905(6) 0.894(6) 0.028 Uiso d 1 . . H H30A 1.116(6) 0.885(5) 0.672(8) 0.028 Uiso d 1 . . H H30B 0.897(9) 0.804(5) 0.627(7) 0.028 Uiso d 1 . . H 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 C1 0.042(6) 0.030(5) 0.029(5) 0.005(4) -0.004(4) -0.004(4) C2 0.049(6) 0.043(6) 0.021(5) 0.001(5) -0.015(4) -0.010(4) C3 0.045(6) 0.040(6) 0.022(5) 0.003(5) -0.015(4) -0.005(4) C5 0.053(7) 0.027(5) 0.035(6) 0.012(5) -0.010(5) 0.007(4) C6 0.050(6) 0.032(6) 0.026(5) -0.001(5) 0.002(5) 0.006(4) C8 0.049(6) 0.027(5) 0.029(5) 0.003(5) 0.012(5) 0.002(4) C9 0.032(5) 0.036(6) 0.037(6) 0.011(4) 0.007(4) 0.007(5) C10 0.046(6) 0.029(5) 0.037(6) 0.005(5) 0.001(5) -0.001(4) C11 0.048(7) 0.042(6) 0.042(6) 0.020(5) -0.006(5) 0.002(5) C12 0.041(6) 0.042(6) 0.036(6) 0.018(5) -0.022(5) -0.004(5) C41 0.040(6) 0.037(6) 0.037(6) 0.008(5) -0.009(5) -0.008(5) C42 0.037(6) 0.038(6) 0.055(7) 0.013(5) 0.006(5) -0.002(5) C71 0.063(8) 0.039(6) 0.024(5) 0.004(6) -0.007(5) 0.009(5) C72 0.055(7) 0.053(7) 0.024(5) 0.014(6) -0.011(5) 0.000(5) C100 0.034(5) 0.035(6) 0.029(5) -0.004(4) -0.005(4) -0.005(4) C111 0.056(7) 0.041(6) 0.024(5) -0.001(5) -0.005(5) 0.011(5) C112 0.034(5) 0.039(6) 0.020(5) -0.004(4) -0.003(4) -0.006(4) N1 0.030(4) 0.045(5) 0.012(4) 0.004(4) -0.002(3) 0.006(3) N4 0.030(4) 0.031(4) 0.027(4) 0.004(3) -0.005(3) 0.001(3) N7 0.033(4) 0.033(5) 0.024(4) 0.005(4) -0.002(3) 0.009(3) N10 0.029(4) 0.032(4) 0.019(4) 0.006(3) 0.003(3) 0.005(3) N11 0.055(6) 0.043(6) 0.037(6) 0.002(5) 0.005(5) -0.007(4) N12 0.048(6) 0.047(6) 0.027(5) 0.012(5) -0.004(4) -0.004(4) N13 0.042(6) 0.075(8) 0.038(6) 0.004(5) -0.008(5) -0.021(5) O1 0.042(4) 0.052(5) 0.033(4) 0.013(4) 0.001(3) -0.003(4) O2 0.053(5) 0.061(6) 0.032(4) 0.003(4) 0.017(4) 0.005(4) O1W 0.154(14) 0.053(7) 0.076(9) 0.003(8) -0.016(9) 0.017(6) O11 0.040(4) 0.044(5) 0.035(4) 0.004(4) 0.008(3) -0.006(4) O12 0.046(5) 0.033(4) 0.044(5) -0.006(4) 0.005(4) -0.009(3) O41 0.050(5) 0.067(6) 0.044(5) 0.035(5) -0.024(4) -0.016(4) O42 0.041(5) 0.058(6) 0.103(9) 0.024(5) -0.009(5) -0.023(6) O71 0.042(4) 0.046(5) 0.028(4) 0.001(4) -0.014(3) -0.004(3) O72 0.068(6) 0.076(7) 0.041(5) 0.008(5) -0.033(5) -0.001(5) Tl1 0.0256(2) 0.0279(2) 0.0160(2) 0.00562(15) -0.00301(14) 0.00037(14) #============================================================================== # 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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 N13 . 1.302(16) ? C1 N11 . 1.312(16) ? C1 N12 . 1.336(14) ? C2 N1 . 1.452(14) ? C2 C3 . 1.533(16) ? C2 H2A . 0.97 ? C2 H2B . 0.97 ? C3 N4 . 1.489(13) ? C3 H3A . 0.97 ? C3 H3B . 0.97 ? C5 N4 . 1.450(14) ? C5 C6 . 1.517(17) ? C5 H5A . 0.97 ? C5 H5B . 0.97 ? C6 N7 . 1.458(14) ? C6 H6A . 0.97 ? C6 H6B . 0.97 ? C8 N7 . 1.462(15) ? C8 C9 . 1.519(16) ? C8 H8A . 0.97 ? C8 H8B . 0.97 ? C9 N10 . 1.463(13) ? C9 H9A . 0.97 ? C9 H9B . 0.97 ? C10 N10 . 1.480(14) ? C10 C100 . 1.507(16) ? C10 H10C . 0.97 ? C10 H10D . 0.97 ? C11 N10 . 1.460(14) ? C11 C12 . 1.523(16) ? C11 H11A . 0.97 ? C11 H11B . 0.97 ? C12 N1 . 1.485(15) ? C12 H12A . 0.97 ? C12 H12B . 0.97 ? C41 N4 . 1.461(15) ? C41 C42 . 1.543(17) ? C41 H41A . 0.97 ? C41 H41B . 0.97 ? C42 O42 . 1.222(15) ? C42 O41 . 1.255(15) ? C71 N7 . 1.484(15) ? C71 C72 . 1.489(18) ? C71 H71A . 0.97 ? C71 H71B . 0.97 ? C72 O72 . 1.231(15) ? C72 O71 . 1.307(15) ? C100 O12 . 1.245(13) ? C100 O11 . 1.262(14) ? C111 N1 . 1.469(14) ? C111 C112 . 1.533(18) ? C111 H11C . 0.97 ? C111 H11D . 0.97 ? C112 O2 . 1.226(14) ? C112 O1 . 1.283(14) ? N1 Tl1 . 2.454(8) ? N4 Tl1 . 2.497(9) ? N7 Tl1 . 2.443(8) ? N10 Tl1 . 2.458(9) ? N11 H10B . 0.91(3) ? N11 H10A . 0.91(3) ? N11 H10B . 0.91(3) ? N12 H20A . 0.90(4) ? N12 H20B . 0.92(3) ? N13 H30A . 0.90(3) ? N13 H30B . 0.91(3) ? O1 Tl1 . 2.322(8) ? O1W H1A . 0.85(2) ? O1W H1B . 0.86(2) ? O11 Tl1 . 2.438(8) ? O41 Tl1 . 2.383(8) ? O71 Tl1 . 2.316(7) ? 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 N13 C1 N11 120.0(10) . . ? N13 C1 N12 120.5(11) . . ? N11 C1 N12 119.5(11) . . ? N1 C2 C3 112.6(9) . . ? N1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? N1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? N4 C3 C2 111.5(9) . . ? N4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? N4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108 . . ? N4 C5 C6 112.5(9) . . ? N4 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? N4 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N7 C6 C5 114.4(10) . . ? N7 C6 H6A 108.7 . . ? C5 C6 H6A 108.7 . . ? N7 C6 H6B 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? N7 C8 C9 113.6(9) . . ? N7 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? N7 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? N10 C9 C8 111.5(9) . . ? N10 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? N10 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 108 . . ? N10 C10 C100 112.2(9) . . ? N10 C10 H10C 109.2 . . ? C100 C10 H10C 109.2 . . ? N10 C10 H10D 109.2 . . ? C100 C10 H10D 109.2 . . ? H10C C10 H10D 107.9 . . ? N10 C11 C12 112.7(9) . . ? N10 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? N10 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N1 C12 C11 112.9(9) . . ? N1 C12 H12A 109 . . ? C11 C12 H12A 109 . . ? N1 C12 H12B 109 . . ? C11 C12 H12B 109 . . ? H12A C12 H12B 107.8 . . ? N4 C41 C42 112.7(9) . . ? N4 C41 H41A 109.1 . . ? C42 C41 H41A 109.1 . . ? N4 C41 H41B 109.1 . . ? C42 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? O42 C42 O41 127.4(13) . . ? O42 C42 C41 115.8(12) . . ? O41 C42 C41 116.7(10) . . ? N7 C71 C72 114.1(10) . . ? N7 C71 H71A 108.7 . . ? C72 C71 H71A 108.7 . . ? N7 C71 H71B 108.7 . . ? C72 C71 H71B 108.7 . . ? H71A C71 H71B 107.6 . . ? O72 C72 O71 124.5(12) . . ? O72 C72 C71 116.7(12) . . ? O71 C72 C71 118.8(10) . . ? O12 C100 O11 124.7(11) . . ? O12 C100 C10 116.8(10) . . ? O11 C100 C10 118.5(9) . . ? N1 C111 C112 112.9(10) . . ? N1 C111 H11C 109 . . ? C112 C111 H11C 109 . . ? N1 C111 H11D 109 . . ? C112 C111 H11D 109 . . ? H11C C111 H11D 107.8 . . ? O2 C112 O1 124.9(11) . . ? O2 C112 C111 116.9(11) . . ? O1 C112 C111 118.2(9) . . ? C2 N1 C111 109.4(9) . . ? C2 N1 C12 112.1(9) . . ? C111 N1 C12 111.7(10) . . ? C2 N1 Tl1 110.2(7) . . ? C111 N1 Tl1 104.2(6) . . ? C12 N1 Tl1 108.9(6) . . ? C5 N4 C41 111.4(9) . . ? C5 N4 C3 110.9(9) . . ? C41 N4 C3 110.7(9) . . ? C5 N4 Tl1 110.1(7) . . ? C41 N4 Tl1 104.6(6) . . ? C3 N4 Tl1 108.9(6) . . ? C6 N7 C8 111.6(9) . . ? C6 N7 C71 111.5(9) . . ? C8 N7 C71 112.0(9) . . ? C6 N7 Tl1 109.6(6) . . ? C8 N7 Tl1 109.1(6) . . ? C71 N7 Tl1 102.6(7) . . ? C11 N10 C9 109.5(9) . . ? C11 N10 C10 110.9(9) . . ? C9 N10 C10 110.2(8) . . ? C11 N10 Tl1 110.5(7) . . ? C9 N10 Tl1 109.9(6) . . ? C10 N10 Tl1 105.7(6) . . ? H10B N11 C1 102(2) . . ? H10B N11 H10A 145(6) . . ? C1 N11 H10A 113(6) . . ? H10B N11 H10B 0(7) . . ? C1 N11 H10B 102(2) . . ? H10A N11 H10B 145(6) . . ? C1 N12 H20A 114(7) . . ? C1 N12 H20B 102(7) . . ? H20A N12 H20B 143(8) . . ? C1 N13 H30A 104(7) . . ? C1 N13 H30B 110(7) . . ? H30A N13 H30B 146(8) . . ? C112 O1 Tl1 115.7(7) . . ? H1A O1W H1B 119(10) . . ? C100 O11 Tl1 114.4(7) . . ? C42 O41 Tl1 118.6(8) . . ? C72 O71 Tl1 113.3(7) . . ? O71 Tl1 O1 112.4(3) . . ? O71 Tl1 O41 73.2(3) . . ? O1 Tl1 O41 73.6(3) . . ? O71 Tl1 O11 75.3(3) . . ? O1 Tl1 O11 72.6(3) . . ? O41 Tl1 O11 119.3(3) . . ? O71 Tl1 N7 70.6(3) . . ? O1 Tl1 N7 159.0(3) . . ? O41 Tl1 N7 88.2(3) . . ? O11 Tl1 N7 126.8(3) . . ? O71 Tl1 N1 159.3(3) . . ? O1 Tl1 N1 70.1(3) . . ? O41 Tl1 N1 125.4(3) . . ? O11 Tl1 N1 86.5(3) . . ? N7 Tl1 N1 115.0(3) . . ? O71 Tl1 N10 90.1(3) . . ? O1 Tl1 N10 126.4(3) . . ? O41 Tl1 N10 158.6(3) . . ? O11 Tl1 N10 67.0(3) . . ? N7 Tl1 N10 73.4(3) . . ? N1 Tl1 N10 73.6(3) . . ? O71 Tl1 N4 126.6(3) . . ? O1 Tl1 N4 90.3(3) . . ? O41 Tl1 N4 67.9(3) . . ? O11 Tl1 N4 157.0(3) . . ? N7 Tl1 N4 72.9(3) . . ? N1 Tl1 N4 73.0(3) . . ? N10 Tl1 N4 115.1(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1A O12 0.85(2) 2.06(5) 2.865(16) 158(11) 1_665 O1W H1B O42 0.86(2) 1.98(5) 2.801(17) 159(11) 1_655 N11 H10B O72 0.91(3) 2.17(4) 3.055(14) 163(3) 2_666 N11 H10B O1W 0.91(3) 2.79(4) 2.95(2) 91(3) 1_455 N12 H20A O11 0.90(4) 2.10(4) 2.961(14) 159(6) 1_665 N12 H20B O2 0.92(3) 2.18(4) 3.063(14) 161(7) 2_667 N13 H30A O12 0.90(3) 2.03(6) 2.844(15) 149(8) 1_665 N13 H30A O11 0.90(3) 2.61(5) 3.449(14) 155(8) 1_665 N13 H30B O72 0.91(3) 1.87(4) 2.777(15) 170(9) 2_666 N11 H10B O1W 0.91(3) 2.79(4) 2.95(2) 91(3) 1_455 C3 H3B O42 0.97 2.29 3.241(17) 165.6 1_655 C5 H5B O72 0.97 2.62 3.379(15) 135.3 2_666 C6 H6B O42 0.97 2.41 3.300(16) 152.6 1_655 C8 H8B O12 0.97 2.47 3.423(14) 167.8 2_656 C9 H9B O41 0.97 2.44 3.296(15) 146.8 1_655 C10 H10D O12 0.97 2.56 3.517(15) 169 2_656 C111 H11C O1W 0.97 2.63 3.470(19) 145.5 2_767 O1W H1A O12 0.85(2) 2.06(5) 2.865(16) 158(11) 1_665 O1W H1B O42 0.86(2) 1.98(5) 2.801(17) 159(11) 1_655 N11 H10A O2 0.91(3) 2.01(4) 2.887(14) 159(8) 2_667 N11 H10B O72 0.91(3) 2.17(4) 3.055(14) 163(3) 2_666 N12 H20A O11 0.90(4) 2.10(4) 2.961(14) 159(6) 1_665 N12 H20B O2 0.92(3) 2.18(4) 3.063(14) 161(7) 2_667 N13 H30A O11 0.90(3) 2.61(5) 3.449(14) 155(8) 1_665 N13 H30A O12 0.90(3) 2.03(6) 2.844(15) 149(8) 1_665 N13 H30B O72 0.91(3) 1.87(4) 2.777(15) 170(9) 2_666 # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF